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Helium gas flow cryostat

Manufactured by Oxford Instruments
Sourced in United Kingdom

The Helium-gas flow cryostat is a laboratory instrument used to precisely control and maintain low temperatures for various applications. It provides a stable and consistent flow of helium gas to create a cryogenic environment suitable for experiments and sample analysis.

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4 protocols using helium gas flow cryostat

1

CW-EPR Spectroscopy of Frozen Samples

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The cw-EPR measurements were performed at 9.7 GHz using an ELEXYS E680 spectrometer (Bruker, Rheinstetten, Germany) with a rectangular cavity (ER 4102 ST), using a modulation frequency of 100 kHz. For measurements at 120 K, a helium-gas flow cryostat (Oxford Instruments, United Kingdom) with an ITC502 temperature controller (Oxford Instruments, United Kingdom) was used. The frozen samples were inserted in the pre-cooled helium-gas flow cryostat. The EPR spectra were recorded using modulation amplitude of 0.25 mT and a microwave power of 0.63 mW. Typical accumulation times were 10–14 min. No absolute calibration of g values was made. For the simulation a constant shift was applied to the B0 field to account for the difference between measured B0 values and the actual B0 values at the sample.
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2

EPR Spectroscopy of Magnetic Samples

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The X-band continuous wave (cw) EPR measurements have been performed using a. an EMX PLUS EPR spectrometer (Bruker, Rheinstetten, Germany) with a super high Q cavity (ER 4119 HS-W1) for room temperature measurements and b. an ELEXSYS E680 spectrometer (Bruker, Rheinstetten, Germany) with a rectangular cavity (ER 4102 ST) for low temperature measurements. The room temperature measurements were done at 20°C, using 0.6315 mW of microwave power, 100 kHz modulation frequency and a modulation amplitude of 1.0 G. Total time to acquire EPR spectra was 20 min. The low-temperature measurements were done at 120 K using a helium gas-flow cryostat (Oxford Instruments, United Kingdom) with an ITC502 temperature controller (Oxford Instruments). The EPR spectra were acquired using a modulation amplitude of 2.5 G and a microwave power of 0.6315 mW.
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3

Continuous Wave EPR Experiments

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Continuous wave (cw) X−band (9–10 GHz) EPR experiments were carried out with Bruker ELEXSYS E580 and ELEXSYS E500 II EPR spectrometers (Bruker Biospin, Rheinstetten, Germany), equipped with an Bruker ER4102ST resonator, ER4122SHQE resonator, or Flexline dielectric ring resonator (Bruker ER 4118X-MD5-W1). Helium gas-flow cryostats (Oxford Instruments and ICE Oxford, UK) and an ITC (Oxford Instruments, UK) were used for cryogenic temperatures. Light excitation was done directly in the resonator with 532 nm Laser light (Nd:YAG Laser, INDI, Newport) or with a white light LED (Thorlabs).
High frequency (HF) EPR measurements were performed on a home-built D-band (130 GHz) spectrometer equipped with a single mode TE011 cylindrical cavity.51 –52 (link) D-band EPR spectra were recorded in pulse mode in order to remove the microwave phase distortion due to fast-passage effects at low temperatures. Light excitation was done directly in the cavity of the spectrometer with 532 nm Laser light through an optical fiber (Nd:YAG Laser, INDI, Newport). Data processing was done using Xepr (Bruker BioSpin, Rheinstetten) and MatlabTM 7.11.2 (MathWorks, Natick) environment. Simulations of the EPR spectra were performed using the EasySpin software package.53 (link)
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4

Nitroxide CW and Pulse EPR Spectroscopy

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X-band CW EPR spectra (microwave (mw) frequency of 9.5 GHz) were measured with a Bruker E500 spectrometer equipped with a variable temperature unit that was operated with liquid N2. The experimental conditions for the CW EPR measurements were as follows: modulation frequency 100 kHz; modulation amplitude 0.03–0.05 mT; mw power 1 mW.
All pulse EPR experiments were done at a temperature of 50 K using helium gas-flow cryostats from Oxford Instruments installed in a Bruker E580 spectrometer (Rheinstetten, Germany, mw frequency 9.8 GHz) equipped with a dielectric resonator MD5, also from Bruker.
HYSCORE experiments were performed with the standard pulse sequence π/2-τ-π/2-π-t1-π–t2–π/2-τ-echo [15 ]. Pulse lengths, unless stated otherwise, were 24 ns for the π/2 pulses and 16 ns for the π pulse. The value of the delay τ was typically 128 ns, as this is a blind spot for the otherwise dominating proton matrix peak. Time delays t1 and t2 were typically varied in steps of 16 ns. The whole sequence was repeated with rates between 250 and 1000 Hz, and an eight-step phase-cycle [15 ] was used to eliminate unwanted echoes. The value of the magnetic field was set to the centre line of the nitroxide spectrum in order to achieve maximum excitation. No orientation selection occurs under these conditions.
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