Determining nanoparticle size in real time by small-angle X-ray scattering in a microscale flow system

Journal of Physical Chemistry C

Volumn 114, Issue 50, 2010, Pages 22055-22063

  McKenzie, Lallie C ^a   Haben, Patrick M ^a   Kevan, Stephen D ^a   Hutchison, James E ^a  

^a UNIVERSITY OF OREGON   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

ANALYTICAL APPROACH; AU NANOPARTICLE; CORE SIZE; EX SITU; FLOW SYSTEMS; IN-SITU; IN-SITU MEASUREMENT; LIGAND-STABILIZED; MICROSCALE FLOW SYSTEM; MICROSCALE SYSTEMS; MULTI-TECHNIQUE APPROACH; NANO-MATERIALS; NANOPARTICLE SIZES; REAL TIME; REAL TIME MEASUREMENTS; SMALL ANGLE X-RAY SCATTERING; TEM; TEM ANALYSIS; UV-VIS SPECTROSCOPY;

FLOWING WELLS; NANOPARTICLES; POLYDISPERSITY; SCATTERING; ULTRAVIOLET SPECTROSCOPY; X RAY SCATTERING;

GOLD;

EID: 79951627250     PISSN: 19327447     EISSN: 19327455     Source Type: Journal    
DOI: 10.1021/jp1077533     Document Type: Article

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47. Residence times in flow systems depend upon both the flow rate and the volume of solution required to fill the tubing between the mixer and the observation cell. In these studies, total flow rates between 0.125 and 4.8 mL/min were used, and the minimum system volume was determined to be 112 μ L (0.57 μ L within the mixer, 46.3 μ Lin4″ of 0.030″ i.d. tubing, and 65 μ L within the observation cell). The shortest residence time accessible was calculated using the highest flow rate, and the longest residence time was calculated using the lowest flow rate. The shortest accessible residence time (1.4 s) was limited by the minimum system volume, while the longest accessible residence time was limited by the volume of sample solution that could be introduced in the system. When combining reagents in a T mixer from two 1 mL syringes and using a flow rate of 0.125 mL/min, a maximum theoretical residence time of 16 min can be accessed. In practice, this residence time is reduced by the length of the data acquisition time and any equilibration period. Using the minimum data acquisition time for our studies (2 min) and allowing 30 s for equilibration, a residence time of 13.5 min can be observed. The temporal resolution was defined by the time needed to refresh the solution in the X-ray path and is estimated in the Experimental Section.