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Published by Krieger Pub Co, Melbourne Copyright: Dover Publications In modern DLS experiments, the scattered light spectral distribution is also measured. In these cases, a photomultiplier is the main detector, but the pre- and postphotomultiplier systems differ depending on the frequency change of the scattered light. The detailed procedure of how to use the DLS instrument will be introduced afterwards. For other more challenging samples such as solutions containing large aggregates, bimodal solutions, very dilute samples, very small nanoparticles, heterogeneous samples, or unknown samples, the results given by DLS could not be really reliable, and one must be aware of the strengths and weaknesses of this analytical technique.
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Then, for the sample preparation procedure, one important question is how much materials should be submit, or what is the optimal concentration of the solution. Generally, when doing the DLS measurement, it is important to submit enough amount of material in order to obtain sufficient signal, but if the sample is overly concentrated, then light scattered by one particle might be again scattered by another known as multiple scattering , and make the data processing less accurate.
In order to get high quality DLS data, there are also other issues to be concerned with.
First is to minimize particulate contaminants, as it is common for a single particle contaminant to scatter a million times more than a suspended nanoparticle, by using ultra high purity water or solvents, extensively rinsing pipettes and containers, and sealing sample tightly.
Second is to filter the sample through a 0. Third is to avoid probe sonication to prevent the particulates ejected from the sonication tip, and use the bath sonication in stead.
Now that the sample is readily prepared and put into the sample holder of the instrument, the next step is to actually do the DLS measurement. Generally the DLS instrument will be provided with software that can help you to do the measurement rather easily, but it is still worthwhile to understand the important parameters used during the measurement. Firstly, the laser light source with an appropriate wavelength should be selected.
One should keep in mind that the nm laser is least suitable for blue samples, while the nm laser is least suitable for red samples, since otherwise the sample will just absorb a large portion of the incident light. Then, for the measurement itself, one has to select the appropriate stabilization time and the duration time.
Dynamic Light Scattering - Applications of Photon Correlation Spectroscopy | R. Pecora | Springer
Another important parameter is the temperature of the sample, as many DLS instruments are equipped with the temperature-controllable sample holders, one can actually measure the size distribution of the data at different temperature, and get extra information about the thermal stability of the sample analyzed. Next, as is used in the calculation of particle size from the light scattering data, the viscosity and refraction index of the solution are also needed.
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Finally, to get data with better reliability, the DLS measurement on the same sample will normally be conducted multiple times, which can help eliminate unexpected results and also provide additional error bar of the size distribution data. Although size distribution data could be readily acquired from the software of the DLS instrument, it is still worthwhile to know about the details about the data analysis process.
There are however, a few methods developed to meet this mathematical challenge: linear fit and cumulant expansion for mono-modal distribution, exponential sampling and CONTIN regularization for non-monomodal distribution. Among all these approaches, cumulant expansion is most common method and will be illustrated in detail in this section. And parameters beyond k 3 are seldom used to prevent overfitting the data. Finally, the size distribution can be easily calculated from the decay rate distribution as described in theory section previously.
The curve through the data is a fit of EQ to the data. The dashed curve shows the weighted residuals: the difference of the fit from the data divided by the uncertainty in each point.
Frisken, Appl. Optics , , 40 , Stock Image. Published by Dover Publications Inc. New Condition: New Soft cover. Save for Later. About this Item Language: English.
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2.4: Dynamic Light Scattering
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