Determination of sample temperature and temperature stability with 129Xe NMR

Saunavaara, Jani; Jokisaari, Jukka

doi:10.1016/j.jmr.2006.01.004

Cited by 9 publications

(11 citation statements)

References 14 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…We eliminate the difficulty of precise temperature control of the experiments in different NMR instruments by using the gaseous and solution-state 129 Xe NMR signal as a chemical shift and temperature reference, respectively. 19 Our experiments demonstrate the existence of the direct field dependence of shielding and, hence, verify the prediction by Ramsey.…”

Section: Introductionsupporting

confidence: 86%

“…To this end, we used the 129 Xe chemical shift in solution, d s Xe , as an internal temperature reference (see ESI †), and ensured that d s Co at each magnetic field corresponds to the same d s Xe value. This procedure is based on the extreme sensitivity of d s Xe upon temperature 19 and is done to gain a precise value for t Co . The resonance frequencies of xenon in gas (g) and in solution (s) can be approximately written as…”

Section: Resultsmentioning

confidence: 99%

“…The magnitude of the field Xe chemical shift of xenon in the solution, d s Xe , is used to approximately detect the temperature T. The given temperatures were determined from the equation given in ref. 19. In this case, the sample contained only D-chloroform and xenon gas.…”

Section: Resultsmentioning

confidence: 99%

See 2 more Smart Citations

Direct magnetic-field dependence of NMR chemical shift

Kantola

Lantto

Heinmaa

et al. 2020

Phys. Chem. Chem. Phys.

Self Cite

View full text Add to dashboard Cite

show abstract

Section: Introductionsupporting

confidence: 86%

Section: Resultsmentioning

confidence: 99%

See 1 more Smart Citation

Direct magnetic-field dependence of NMR chemical shift

Kantola

Lantto

Heinmaa

et al. 2020

Phys. Chem. Chem. Phys.

Self Cite

View full text Add to dashboard Cite

show abstract

“…Highly accurate and precise measurements of the sample temperature can be achieved in a non-invasive way by using the temperature-dependence of the chemical shift of suitable nuclei as thermometers (Dickert and Hellmann 1980; Field et al 1984; Hedin and Furo 1998; Quast et al 1998; Sikorski et al 1998; Saunavaara and Jokisaari 2006; Findeisen et al 2007). This is being used in many practical applications, in particular to calibrate the temperature unit of the NMR probe upon installation (van Geet 1970; Bornais and Brownstein 1978; Levy et al 1980; Ammann et al 1982), to map the local temperature in steady and non-steady state conditions (Wimmer and Wider 2007), to detect thermal convection currents (Jerschow 2000), or to improve the temperature stabilization (Keiichiro 1991).…”

Section: Introductionmentioning

confidence: 99%

The T-lock: automated compensation of radio-frequency induced sample heating

2009

View full text Add to dashboard Cite

Modern high-field NMR spectrometers can stabilize the nominal sample temperature at a precision of less than 0.1 K. However, the actual sample temperature may differ from the nominal value by several degrees because the sample heating caused by high-power radio frequency pulses is not readily detected by the temperature sensors. Without correction, transfer of chemical shifts between different experiments causes problems in the data analysis. In principle, the temperature differences can be corrected by manual procedures but this is cumbersome and not fully reliable. Here, we introduce the concept of a "T-lock", which automatically maintains the sample at the same reference temperature over the course of different NMR experiments. The T-lock works by continuously measuring the resonance frequency of a suitable spin and simultaneously adjusting the temperature control, thus locking the sample temperature at the reference value. For three different nuclei, 13 C, 17 O and 31 P in the compounds alanine, water, and phosphate, respectively, the T-lock accuracy was found to be < 0.1 K. The use of dummy scan periods with variable lengths allows a reliable establishment of the thermal equilibrium before the acquisition of an experiment starts.

show abstract

“…Several compounds with temperature-dependent chemical shifts have been reported as NMR-thermometers, involving 1 H, 2 H, 19 F, 13 C, 31 P [7] and 129 Xe [8]. One of the most temperature-sensitive NMR resonances is observed for 59 Co [9], which can easily be measured in highly symmetric complexes like hexacyanocobaltate(III), CoðCNÞ 6 3À .…”

Section: Introductionmentioning

confidence: 99%