High-precision nuclear magnetic resonance probe suitable for in situ studies of high-temperature metallic melts

2022 ◽  
Author(s):  
Ao Li ◽  
Wei Xu ◽  
Xiao Chen ◽  
Bing-Nan Yao ◽  
Jun-Tao Huo ◽  
...  

Abstract High-temperature nuclear magnetic resonance (NMR) has proven to be very useful for detecting the temperature-induced structural evolution and dynamics in melts. However, the sensitivity and precision of high-temperature NMR probes are limited. Here we report a sensitive and stable high-temperature NMR probe based on laser-heating, suitable for in situ studies of metallic melts, which can work stably at the temperature of up to 2000 K. In our design, a well-designed optical path and the use of a water-cooled copper radio-frequency (RF) coil significantly optimize the signal-to-noise ratio (S/NR) at high temperatures. Additionally, a precise temperature controlling system with an error of less than ±1 K has been designed. After temperature calibration, the temperature measurement error is controlled within ±2 K. As a performance testing, 27Al NMR spectra are measured in Zr-based metallic glass-forming liquid in situ. Results show that the S/NR reaches 45 within 90 s even when the sample's temperature is up to 1500 K and that the isothermal signal drift is better than 0.001 ppm per hour. This high-temperature NMR probe can be used to clarify some highly debated issues about metallic liquids, such as glass transition and liquid-liquid transition.

1982 ◽  
Vol 60 (9) ◽  
pp. 917-921 ◽  
Author(s):  
John W. Shriver ◽  
Brian D. Sykes

An enzymatic orthophosphate removal system is described which can be effectively used to continuously remove orthophosphate from biochemical samples. The phosphorolysis of nicotinamide riboside is catalyzed by calf spleen nucleoside phosphorylase to give ribose-1-PO4 and nicotinamide along with a proton. At pH 8 the production of ribose-1-PO4 from orthophosphate is essentially quantitative. This reaction can be monitored optically or by 31P nuclear magnetic resonance (NMR). Equations are given for determining the time required to remove a given amount of phosphate from a typical NMR sample with a known amount of nucleoside phosphorylase. The effects of a competing orthophosphate-producing reaction are considered.


Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1416 ◽  
Author(s):  
Mohamed Haouas

The employment of nuclear magnetic resonance (NMR) spectroscopy for studying crystalline porous materials formation is reviewed in the context of the development of in situ methodologies for the observation of the real synthesis medium, with the aim of unraveling the nucleation and growth processes mechanism. Both liquid and solid state NMR techniques are considered to probe the local environment at molecular level of the precursor species either soluble in the liquid phase or present in the reactive gel. Because the mass transport between the liquid and solid components of the heterogeneous system plays a key role in the synthesis course, the two methods provide unique insights and are complementary. Recent technological advances for hydrothermal conditions NMR are detailed and their applications to zeolite and related materials crystallization are illustrated. Achievements in the field are exemplified with some representative studies of relevance to zeolites, aluminophosphate zeotypes, and metal-organic frameworks.


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