Double resonance mas probe head

Manufactured by Bruker

Sourced in United States, Germany

The Double-resonance MAS probe head is a specialized laboratory equipment designed for solid-state nuclear magnetic resonance (NMR) spectroscopy. Its core function is to enable the simultaneous excitation and detection of multiple nuclear spin species within a sample under magic-angle spinning (MAS) conditions.

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Dsx 400 spectrometer, by Bruker (1 mentions) Avance 400 mhz spectrometer, by Bruker (1 mentions) Avance 400 spectrometer, by Bruker (1 mentions) Avance 3 400 wb spectrometer, by Bruker (1 mentions) Advance 400 spectrometer, by Bruker (1 mentions)

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MAS probe (11 citations)

5 protocols using double resonance mas probe head

Solid-state NMR Analysis of Wet Cellulose

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The pre-wet NMR samples (with approximately 55% water content) were
prepared with isolated cellulose packed into a 4-mm cylindrical ceramic MAS rotor
(Bruker, Billerica, MA, United States). Repetitive steps of packing samples into
the rotor were performed to fully compress and load the maximum amount of sample.
Solid-state NMR measurements were carried out on a Bruker DSX-400 spectrometer
(Bruker, Billerica, MA, United States) operating at frequencies of 100.55 MHz for
carbon-13 in a Bruker double-resonance MAS probe head (Bruker, Billerica, MA,
United States) at spinning speeds of 10 kHz. CP/MAS experiments utilized a 5 μs
(90°) proton pulse, 1.5 ms contact pulse, 4.0 second recycle delay and 4–8 K
scans. All spectra were recorded on wet samples (with approximately 55% water
content), and the line-fitting analysis of spectra was performed using NUTS NMR
Data Processing software (Acorn NMR, Inc., Livermore, CA, United States). Error
analysis was conducted by performing three individual isolations, NMR
acquisitions, and line-fit data processing [59 (link),60 (link)].

Sun Q., Foston M., Meng X., Sawada D., Pingali S.V., O’Neill H.M., Li H., Wyman C.E., Langan P., Ragauskas A.J, & Kumar R. (2014). Effect of lignin content on changes occurring in poplar cellulose ultrastructure during dilute acid pretreatment. Biotechnology for Biofuels, 7, 150.

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Solid-State NMR Analysis of Cellulose Crystallinity

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Solid-state NMR analysis for cellulose crystallinity was performed as previously described with minor modification [20 (link), 33 (link)]. The isolated cellulose samples were stored in a sealed container to prevent moisture loss. The NMR samples were prepared by packing the moisturized cellulose into 4-mm cylindrical Zirconia MAS rotors. Cross-polarization magic angle spinning (CP/MAS) NMR analysis of cellulose was carried out on a Bruker Avance-400 MHz spectrometer operating at frequencies of 100.59 MHz for ¹³C in a Bruker double-resonance MAS probe head at spinning speeds of 8 kHz. CP/MAS experiments utilized a 5-µs (90°) proton pulse, 1.5-ms contact pulse, 4-s recycle delay, and 4000 scans. The cellulose crystallinity index (CrI) was determined from the areas of the crystalline and amorphous C₄ signals using the following formula:

CrI = \frac{A_{86 - 92 ppm}}{A_{86 - 92 ppm} + A_{79 - 86 ppm}} .

Li M., Cao S., Meng X., Studer M., Wyman C.E., Ragauskas A.J, & Pu Y. (2017). The effect of liquid hot water pretreatment on the chemical–structural alteration and the reduced recalcitrance in poplar. Biotechnology for Biofuels, 10, 237.

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Cellulose Crystallinity Analysis by Solid-State NMR

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Cellulose crystallinity was measured with cross‐polarization magic angle spinning (CP/MAS) solid‐state NMR according to published procedure (Li et al., 2017). Cellulose for solid‐sate NMR analysis was isolated from the holocellulose (150 mg) by hydrolysis at 100 °C with HCl (8 mL of 2.5 m) for 2 h. The isolated cellulose was retained at 30%–50% moisture. The NMR samples were packed into 4‐mm cylindrical Zirconia MAS rotors. CP/MAS NMR analysis of cellulose was carried out on a Bruker Avance‐400 spectrometer operating at frequencies of 100.59 MHz for ¹³C in a Bruker double‐resonance MAS probe head at spinning speeds of 8 kHz. CP/MAS experiments utilized a 5 ms (90 °) proton pulse, 1.5 ms contact pulse, 4 s recycle delay and 2048 scans. The cellulose crystallinity index (CrI) was determined from the areas of the crystalline and amorphous C‐4 signals using the following formula:

\frac{A_{86 - 92 ppm}}{A_{86 - 92 ppm} + A_{79 - 86 ppm}}

Zhang J., Xie M., Li M., Ding J., Pu Y., Bryan A.C., Rottmann W., Winkeler K.A., Collins C.M., Singan V., Lindquist E.A., Jawdy S.S., Gunter L.E., Engle N.L., Yang X., Barry K., Tschaplinski T.J., Schmutz J., Tuskan G.A., Muchero W, & Chen J. (2019). Overexpression of a Prefoldin β subunit gene reduces biomass recalcitrance in the bioenergy crop Populus. Plant Biotechnology Journal, 18(3), 859-871.

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Cellulose Isolation and Characterization

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The crystallinity and crystal forms of the cellulose were characterized by solid-state cross-polarization/magic angle spinning (CP/MAS) ¹³C NMR. Cellulose was isolated according to the following protocol, as modified from a previous procedure [26 (link)]; Briefly, the fiber samples (9 g) were dispersed into 750 mL of deionized water. Then glacial acetic acid (6 mL) and sodium chlorite (6 g) were added to the mixture. The mixture was sealed in a reaction flask and maintained at 70 °C with stirring for 2 h. This treatment was repeated until the solid residue turned white and the lignin content was very low. After that, cellulose was isolated from 2 g of solid residue by soaking in 200 mL of 2.5 M HCl at 100 °C for 4 h and was then filtered and washed with deionized water.
Solid-state NMR measurements were carried out on a AVANCE III 400 WB spectrometer (Bruker, Germany) operating at a frequency of 100.69 MHz for ¹³C using a 4-mm Bruker double-resonance MAS probe head at a spinning speed of 10 kHz. Acquisition was performed with a CP pulse sequence using a 2.5-µs proton 90° pulse, a 1.5-ms contact pulse, and a 3.0-s delay between repetitions.

Lü F., Chai L., Shao L, & He P. (2017). Precise pretreatment of lignocellulose: relating substrate modification with subsequent hydrolysis and fermentation to products and by-products. Biotechnology for Biofuels, 10, 88.

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Cellulose Crystallinity Analysis by Solid-State NMR

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Solid-state NMR analysis for cellulose crystallinity was performed as described previously with minor modification [42 (link)]. The isolated cellulose samples were stored in a sealed container to prevent moisture loss. The NMR samples were prepared by packing the moisturized cellulose into 4-mm cylindrical Zirconia MAS rotors. Cross-polarization magic angle spinning (CP/MAS) NMR analysis of cellulose was carried out on a Bruker Advance-400 spectrometer operating at a frequency of 100.59 MHz for ¹³C in a Bruker double-resonance MAS probe head at the spinning speed of 10 kHz. CP/MAS experiments utilized a 5 µs (90°) proton pulse, 1.5 ms contact pulse, 4 s recycle delay, and 4000 scans. The cellulose crystallinity index (CrI) was determined from the areas of the crystalline and amorphous C₄ signals using the following formula:

CrI = \frac{A_{86 - 92 ppm}}{A_{86 - 92 ppm} + A_{79 - 86 ppm}} .

Li M., Pu Y., Yoo C.G., Gjersing E., Decker S.R., Doeppke C., Shollenberger T., Tschaplinski T.J., Engle N.L., Sykes R.W., Davis M.F., Baxter H.L., Mazarei M., Fu C., Dixon R.A., Wang Z.Y., Neal Stewart C J.r, & Ragauskas A.J. (2017). Study of traits and recalcitrance reduction of field-grown COMT down-regulated switchgrass. Biotechnology for Biofuels, 10, 12.

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