Gradient techniques calibration

An entirely different type of transport is formed by thermal convection and conduction. Flow induced by thermal convection can be examined by the phaseencoding techniques described above [8, 44, 45] or by time-of-flight methods [28, 45]. The latter provide less quantitative but more illustrative representations of thermal convection rolls. The origin of any heat transport, namely temperature gradients and spatial temperature distributions, can also be mapped with the aid of NMR techniques. Of course, there is no direct encoding method such as those for flow parameters. However, there are a number of other parameters, for example, relaxation times, which strongly depend on the temperature so that these parameters can be calibrated correspondingly. Examples are described in Refs. [8, 46, 47], for instance. 

Several techniques are available for thermal conductivity measurements, in the steady state technique a steady state thermal gradient is established with a known heat source and efficient heat sink. Since heat losses accompany this non-equilibrium measurement the thermal gradient is kept small and thus carefully calibrated thermometers and heat source must be used. A differential thermocouple technique and ac methods have been used. Wire connections to the sample can represent a perturbation to the measurement. Techniques with pulsed heat sources (including laser pulses) have been used in these cases the dynamic response interpretation is more complicated. 

Load the spectrum of the gradient-assisted, inverse detected, 2D CH-HSQC-TOCSY experiment acquired with the echo-antiecho technique, D NMRDATA GLUCOSE 2D CH GCHICOTO 001999.RR. Check and if necessary correct its calibration in both dimensions. Set up a layout as for the basic HSQC spectrum. Compare the spectrum with the spectra of the basic HSQC and HMQC experiments. Use the same rows or columns to identify the additional TOCSY-peaks. 

Carbon-14 content is measured by specially designed gas proportional counters (7. Aerosol samples are first converted to CO2 by combustion in a macroscale version of the thermal evolution technique. A clam shell oven was used to heat the sample for sequential evolution of organic and elemental carbon under equivalent conditions. Due to the possibility of thermal gradients, conditions in the macroscale apparatus were adjusted to produce the same recoveries of total carbon (yg C per cm of filter area) as for the microscale apparatus. Carbon-14 data are reported as % contemporary carbon based on the 1978 1 C02 content in the atmosphere. Aldehyde data referred to in this paper were obtained by impinger sampling in dinitrophenylhydrazine/acetonitrile solution and analysis of the derivatives by HPLC with UV detection (12). Olefin measurements were made by a specially designed ozone-chemiluminescence apparatus (13) difficulties in calibration accuracy and background drift with temperature limit its use to inferences of relative reactive hydrocarbon levels. 

Because H linewidths in many elastomers are of the order of 3 kHz or less, spin-echo and gradient-echo imaging techniques can be applied. Contrast is introduced by suitable filters like Ti and double-quantum filters or by use of the spectroscopic dimension. Parameter images of T2, the double-quantum signal intensity, or the quadrupolar coupling strength are evaluated and rescaled according to theory or experimental calibration data (cf. Section 7.1.6). 

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