I want to take DLS measurements of iron oxide nanoparticles. But most of the time, particles were not able to disperse in water by ultrasonication. Can anyone suggest me, how to prepare sample for DLS measurements.
Ankur Verma If you're starting with a powder then it's a laser diffraction experiment, not DLS. You have no free, independent, discrete particles < 100 nm in a powder. For further information, please view this webinar (free registration required):
If water is not working as a dispersion medium even after sonication then try to change the dispersion medium to alcohols(ethanol) etc. But before that, as you have not mentioned sonication time I assume you at least sonicate it for a minimum of 30 min if not increase it to a maximum of an hour. Then go for an alternate dispersion medium. Also, check your water's pH before and after adding your nanoparticles to make sure it's almost near neutral with + or - 1 acceptable(i.e 6,7,8). Also, take your nanoparticle dispersion in low concentration (1mg/100ml) or even lesser concentration.
Aravindhan Vanangamudi There is a 'comminution limit'. Sonicating for 30 - 60 minutes with a probe sonicator will contaminate the suspension as the tip disintegrates (if you don't believe me then try sonicating 18 M-Ohm water in such a manner and measuring the conductivity over time). Sonication can also promote aggregation and agglomeration. In organic solvents most of the ultrasound energy is used in boiling the solvent and converting it to vapor. Water is the best medium for transmitting ultrasound energy.
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'I think dry nanotechnology is probably a dead-end' Rudy Rucker Transhumanity Magazine (August 2002)
‘If the particles are agglomerated and sub-micron it may be impossible to adequately disperse the particles……‘The energy barrier to redispersion is greater if the particles have been dried. Therefore the primary particles must remain dispersed in water….’ J H Adair, E. Suvaci, J Sindel, “Surface and Colloid Chemistry” Encyclopedia of materials: Science and Technology pp 8996 - 9006 Elsevier Science Ltd. 2001 ISBN 0-08-0431526
‘The energy barrier to redispersion is greater if the particles have been dried. Therefore the primary particles must remain dispersed in water….’
Once your system is dried you cannot easily return to the dispersed state - the same situation as the drained marshes in Iraq. Simply adding water back into the system does not regenerate the habitat... See: https://www.rferl.org/a/1104940.html
Accurate DLS measurements require that the nanoparticles are well-dispersed in solution to avoid aggregation and obtain reliable results.
In the case of iron oxide nanoparticles, ultrasonication is often used to disperse the particles in solution. However, if ultrasonication is not sufficient to disperse the nanoparticles, you can try the following steps to prepare a sample for DLS measurements:
Choose an appropriate dispersant: The choice of a suitable dispersant is critical for the successful dispersion of nanoparticles. In the case of iron oxide nanoparticles, commonly used dispersants include water, ethanol, and organic solvents such as acetone or chloroform.
Choose an appropriate concentration: The concentration of nanoparticles can affect the stability and dispersion of the particles in solution. It is recommended to start with a low concentration (e.g., 0.1 mg/mL) and increase the concentration gradually if necessary.
Use a surfactant: The addition of a surfactant such as Tween 20 or Triton X-100 can help to stabilize the nanoparticles and prevent aggregation.
Sonicate the sample: Ultrasonication is often used to disperse nanoparticles in solution. Sonicate the sample for a sufficient time (e.g., 5-10 minutes) with short intervals to prevent sample heating.
Filter the sample: After sonication, it is recommended to filter the sample through a 0.2 µm filter to remove any residual aggregates or large particles.
Avoid air bubbles: To avoid air bubbles, vortex the sample gently for a short time to remove any bubbles and ensure the sample is homogeneous.
By following these steps, you should be able to prepare a well-dispersed sample of iron oxide nanoparticles for DLS measurements. It's important to note that the appropriate sample preparation may depend on the specific properties of the nanoparticles and the dispersant used. Therefore, it's recommended to optimize the preparation method for your specific case
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