International
Tables for
Crystallography
Volume C
Mathematical, physical and chemical tables
Edited by E. Prince

International Tables for Crystallography (2006). Vol. C. ch. 2.6, p. 109

Section 2.6.2.6.3. Estimation of the incoherent scattering level

R. Mayb

2.6.2.6.3. Estimation of the incoherent scattering level

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For an exact knowledge of the scattering curve, it is necessary to subtract the level of incoherent scattering from the scattering curve, which is initially a superposition of the (desired) coherent sample scattering, electronic and neutron background noise, and (sometimes dominant) incoherent scattering.

A frequently used technique is the subtraction of a reference sample that has the same level of incoherent scattering, but lacks the coherent scattering from the inhomogeneities under study. Although this seems simple in the case of solutions, in practice there are problems: Very often, the 1H/2H mixture is made by dialysis, and the last dialysis solution is taken as the reference. The dialysis has to be excessive to obtain really identical levels of 1H, and in reality there is often a disagreement that is more important the lower the sample concentration is. If the concentration is high, then the incoherent scattering from the sample atoms (protons) themselves becomes important.

For dilute aqueous solutions, there is a procedure using the sample and reference transmissions for estimating the incoherent background level (May, Ibel & Haas, 1982[link]): The incoherent scattering level from the sample, [I_{i,s}], can be estimated as [I_{i,s}=I[{\rm H_2O}]\,f_\lambda (1-T_s)/(1-T[{\rm H_2O}]),\eqno (2.6.2.9)]where [I[{\rm H_2O}]] is the scattering from a water sample, [T[{\rm H_2O}]] is transmission, [T_s] that of the sample. [f_\lambda] is a factor depending on the wavelength, the detector sensibility, the solvent composition, and the sample thickness; it can be determined experimentally by plotting Ii,s/I[H2O] versus (1 − Ts)/(1 − T[H2O]) for a number of partially deuterated solvent mixtures.

This procedure is justified because of the overwhelming contribution of the incoherent scattering of 1H to the macroscopic scattering cross section of the solution, and therefore to its transmission. The procedure should also be valid for organic solvents. The precision of the estimation is limited by the precision of the transmission measurement, the relative error of which can hardly be much better than about 0.005 for reasonable measuring times and currently available equipment, and by the (usually small) contribution of the coherent cross section to the total cross section of the solution. A modified version of (2.6.2.9)[link] can be used if a solvent with a transmission close to that of a sample has been measured, but the factor [f_\lambda] should not be omitted.

An equation similar to (2.6.2.9)[link] holds for systems with a larger volume occupation c of particles in a (protonated) solvent with a scattering level [I_{\rm inc}] in a cell with identical pathway (without the particles): [I_{i,s}=I_{\rm inc}(1-T^{1-c}_{\rm inc})/(1-T_{\rm inc}).\eqno(2.6.2.9a)]In this approximation, the particles' cross-section contribution is assumed to be zero, i.e. the particles are considered as bubbles.

In the case of dilute systems of monodisperse particles, the residual background (after initial corrections) can be quite well estimated from the zero-distance value of the distance-distribution function calculated by the indirect Fourier transformation of Glatter (1979[link]).

References

First citation Glatter, O. (1979). The interpretation of real-space information from small-angle scattering experiments. J. Appl. Cryst. 12, 166–175.Google Scholar
First citation May, R. P., Ibel, K. & Haas, J. (1982). The forward scattering of cold neutrons by mixtures of light and heavy water. J. Appl. Cryst. 15, 15–19.Google Scholar








































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