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7 mm cpmas probe

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The 7 mm CPMAS probe is a laboratory equipment used for solid-state nuclear magnetic resonance (NMR) spectroscopy. It is designed to operate at a specific radio frequency and accommodate sample sizes up to 7 millimeters in diameter. The probe's core function is to generate and detect the NMR signal from the sample, enabling the analysis of solid-state materials.

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Lab products found in correlation

Avance 400 mhz, by Bruker (2 mentions) 300 mhz spectrometer, by Bruker (1 mentions)

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CPMAS probe (7 citations)

3 protocols using 7 mm cpmas probe

1

Solid-State 13C NMR Spectroscopy Protocol

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Example 6

The solid state 13C NMR spectrum was measured under the following conditions. The results are shown in FIG. 6.

(Measurement Conditions)

Used apparatus: Avance400 MHz (manufactured by BRUKER) 7

mm-CPMAS probe (manufactured by BRUKER)

Measured nucleus: 13C (resonant frequency 100.6248425 MHz)

Measurement temperature: room temperature (22° C.)

Pulse mode: CPTOSS measurement

Rotation number: 5,000 Hz

Pulse repetition time: 4 second

Contact time: 1 millisecond

Number of scans: 8,000

Reference material: glycine (external reference: 176.03 ppm)

The solid state 13C NMR spectrum was obtained by CPTOSS method (a method for eliminating spinning side bands) with carbon nucleus (resonance frequency 100.6 MHz) using an NMR instrument, BRUKER Avance 400 MHz equipped with a 7 mm CPMAS probe (manufactured by BRUKER). The sample tube enclosing approximately 300 mg of a solid sample was rotated at 5 kHz and measured using contact time of 1 millisecond, pulse delay time of 4 second and number of scans of 8000 at room temperature (22° C.). Chemical shifts were corrected by an external reference method with carbonyl carbon of glycine being 176.03 ppm.

US10221183B2. Crystal (6S,9aS)-N-benzyl-8-({6-[3-(4-ethylpiperazin-1-yl)azetidin-1-yl]pyridin-2-yl}methyl)-6-(2-fluoro-4-hydroxybenzyl)-4,7-dioxo-2-(prop-2-en-1-yl)hexahydro-2H-pyrazino[2,1-c][1,2,4]triazine-1(6H)-carboxamide (2019-03-05). Eisai R&D Management Co., Ltd. [JP]. Inventors: Ikuo Kushida [JP], Yoko Ito [JP].
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2

Solid-State 13C NMR Spectroscopy Protocol

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Example 6

The solid state 13C NMR spectrum was measured under the following conditions. The results are shown in FIG. 6.

(Measurement Conditions)

Used apparatus: Avance400 MHz (manufactured by BRUKER) 7

mm-CPMAS probe (manufactured by BRUKER)

Measured nucleus: 13C (resonant frequency 100.6248425 MHz)

Measurement temperature: room temperature (22° C.)

Pulse mode: CPTOSS measurement

Rotation number: 5,000 Hz

Pulse repetition time: 4 second

Contact time: 1 millisecond

Number of scans: 8,000

Reference material: glycine (external reference: 176.03 ppm)

The solid state 13C NMR spectrum was obtained by CPTOSS method (a method for eliminating spinning side bands) with carbon nucleus (resonance frequency 100.6 MHz) using an NMR instrument, BRUKER Avance 400 MHz equipped with a 7 mm CPMAS probe (manufactured by BRUKER). The sample tube enclosing approximately 300 mg of a solid sample was rotated at 5 kHz and measured using contact time of 1 millisecond, pulse delay time of 4 second and number of scans of 8000 at room temperature (22° C.). Chemical shifts were corrected by an external reference method with carbonyl carbon of glycine being 176.03 ppm.

US10259817B2. Crystal (6S,9aS)-N-benzyl-8-({6-[3-(4-ethylpiperazin-1-yl)azetidin-1-yl]pyridin-2-yl}methyl)-6-(2-fluoro-4-hydroxybenzyl)-4,7-dioxo-2-(prop-2-en-1-yl)hexahydro-2H-pyrazino[2,1-c][1,2,4]triazine-1(6H)-carboxamide (2019-04-16). Eisai R&D Management Co., Ltd. [JP]. Inventors: Ikuo Kushida [JP], Yoko Ito [JP].
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3

Solid-state 15N NMR Analysis Protocol

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All solid-state 15N NMR cross-polarization magic-angle spinning (CP-MAS) measurements
were performed at Analytical and Technical Services at SUNY ESF using
a 300 MHz Bruker spectrometer with a 7 mm CPMAS probe with the sample
at 25 °C. The spinning rate was 4000 Hz; acquisition time, 0.02
s; number of data points, 484; delay between pulses, 5 s; sweep width,
400 ppm (12 165.450 Hz); 1H decoupling field, 47 200
Hz; and spectra were processed with a line broadening of 40 Hz. All
chemical shifts are referenced to an ammonium-15N2 sulfate standard (defined as 0 ppm).
Banyikwa A.T., Miller S.E., Krebs R.A., Xiao Y., Carney J.M, & Braiman M.S. (2017). Anhydrous Monoalkylguanidines in Aprotic and Nonpolar Solvents: Models for Deprotonated Arginine Side Chains in Membrane Environments. ACS Omega, 2(10), 7239-7252.
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