2011
DOI: 10.5012/bkcs.2011.32.6.1970
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Convection Effects on PGSE-NMR Self-Diffusion Measurements at Low Temperature: Investigation into Sources of Induced Convective Flows

Abstract: The effects of convection on the measurement of the diffusion coefficients of liquids by the pulsed gradient spin echo (PGSE) NMR method at low temperature are discussed. To examine the generation of convective flows, we used four different types of sample tubes in the diffusion measurements with temperature variation; a normal 5 mm NMR tube, a Shigemi tube, an ELISE type tube, and a capillary tube. Below room temperature, the calculated diffusion coefficients of chloroform in 5 mm o.d. type tubes increased wi… Show more

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Cited by 19 publications
(19 citation statements)
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“…Pure water at 37 °C showed an ADC of D = 3.65 ± 0.05 µm 2 /ms, which is around 25% above literature values and can be attributed to convection effects arising from temperature gradients because of the nitrogen air flow, which keeps samples at a stable temperature inside the NMR spectrometer. Although the whole sample is confined to the coil region and susceptibility plugs were used (see NMR measurements), convective flow is present in thermal 1 H diffusion measurements at both low and high temperatures .…”
Section: Methodsmentioning
confidence: 99%
“…Pure water at 37 °C showed an ADC of D = 3.65 ± 0.05 µm 2 /ms, which is around 25% above literature values and can be attributed to convection effects arising from temperature gradients because of the nitrogen air flow, which keeps samples at a stable temperature inside the NMR spectrometer. Although the whole sample is confined to the coil region and susceptibility plugs were used (see NMR measurements), convective flow is present in thermal 1 H diffusion measurements at both low and high temperatures .…”
Section: Methodsmentioning
confidence: 99%
“…The spectrometer's temperature sensor was calibrated with a platinum resistance thermometer (Pt-100) that was, in turn, calibrated in our laboratory using a certified standard. The standard uncertainty of the temperature measurement is estimated as u(T) = 0.1 K. Special sample tubes with an outer diameter of 2.5 mm (Deutero GmbH, Germany) were used in order to minimize sample convection 41 and radiation damping. 42 A stimulated spin−echo technique with bipolar pulsed gradients 43 was applied as implemented in the NMR spectrometer's software (pulse sequence: stebpgp1s).…”
Section: ■ Experimental Proceduresmentioning
confidence: 99%
“…The stability of the thermostating gas flow is ±0.05 K. The overall uncertainty of the temperature measurement is estimated to be below ±0.15 K. Special NMR sample tubes with a capillary bottom with a bottom outer diameter of 2.5 mm (Deutero GmbH, Germany) were used in order to minimize the convection inside the sample and to reduce radiation damping. [31,32] The stimulated spin-echo technique with bipolar pulsed gradients [33] was applied as implemented in the spectrometer software (Bruker TopSpin 3.2, pulse sequence: stebpgp1s). The self-diffusion coefficient of species i (D i ) is obtained from a fit of the natural logarithm of the relative signal intensity against the squared gradient strength according to Eq.…”
Section: Pfg-nmr Measurementsmentioning
confidence: 99%