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102 IV.2. Mesostructured silica coating in a micro-fabricated-column, ., p.102 ,
, IV.2.1.1. Flow profile simulation through different cross-section geometries
Thicker sol-gel deposition in the corner, IV.2.1.2, p.104 ,
, , p.105
, IV.2.2. Connection capillaries influence on chromatographic results, p.107
, IV.2.2.1. Flow calculation in a column with multiple geometrical components, p.107
Micro-column coating process adaptation, IV.2.2.2 ,
, IV.2.2.3. Process for changing the connections, p.109
, , p.110
, IV.3.2. Capillary connections influence, p.111
, , p.111
Experimental results on entry shortening, IV.3.2.2, p.113 ,
Micro-column's kinetic evaluation, IV.3.3, p.113 ,
, , p.113
Comparison to other published micro-fabricated columns results, IV.3.3.2, p.114 ,
, IV.4. Other chromatographic results, p.116
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Hollow core-shell mesoporous nanoparticles synthesis, p.170 ,
Polystyrene cationic latex synthesis, p.170 ,
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Amino acid catalyzed Mesoporous silica nanoparticles synthesis, p.171 ,
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, Layer-by-layer deposition 5 glass crystallizers were filled with approximately 100 mL of the PAH solution, the LUDOX particles solution and deionized water from PureLab station
, A cycle consists in the following steps, realized under slow orbital stirring (75 rpm): -5 minutes in the PAH solution (15 minutes for the first cycle) -1 minute in each water solution -5 minutes in the LUDOX particles solution (15 minutes for the first cycle) -1 minute in each water solution The water contained in the 3 crystallizers is replaced each time the substrates are in the LUDOX particles or PAH solutions, Silicon substrates were alternately dipped into the crystallizers for several cycles
, A.5.3. Micro-column packing
, An Ordyl® film was laminated onto glass substrate (of the size of the micro-columns chip), and applied under a metal weight (10 kg, distributed between 2 chips) in an oven at 160°C for one night
, Then capillaries are glued at the inlet and outlet of the column with a silicon glue, similarly to micro-columns coated with sol-gel
Poiseuille flow through a capillary column, p.178 ,
, , p.178
, , p.179
, , p.179
Laminar flow through micro-columns, p.180 ,
Velocity profile through a rectangular cross section, p.180 ,
Compressible flow through the micro-column, p.181 ,
Incompressible flow through multiple column segments, p.181 ,
Compressible flow through multiple column segments, p.181 ,
, , p.182
, , p.182
HETP of a column with multiple segments, p.183 ,
, , p.184
, , p.187
, Compressible flow through the micro-column B.3.2.1. Incompressible flow through multiple column segments In addition to their rectangular cross section, one has also to take into account the connection capillaries to calculate the flow and the average velocity of the carrier gas through the column. Each part of the column can be considered as a segment. For each segment i, it is possible to calculate the flow as a function of the pressure drop between its extremities
, 13) is more complicated in the case of the micro-column, and its rectangular cross-section, but it can be calculated as well. As flow conservation is required from one segment to the other, F is constant. Thus, in equation B.12, it is possible to recognize an analogy with an electric circuit of multiple resistor in series, with ?Pi being the tension, and F the intensity. Thus, for a column with 3 segments, The expression of Ri
, Compressible flow through multiple column segments In the case of a compressible flow, it is no more F that is constant but P x F. This changes slightly the equation but analytical solutions are still simple to get
, Where Pi is the pressure at the end of the segment i
, For a rectangular geometry, we used the most recent model from H. Ahn and S
, HETP of a column with multiple segments Another form for H is
, Where tr is the average time for the analyte to go through the column: B
, And ? 2 the dispersion of the peak (i.e. the variance of the Gaussian), assumed to have a
, Gaussian shape. Consequently, the total dispersion of the peak at the end of the column is equal to the sum of the dispersion it acquired in all the segment
, Where: B, vol.27
, And Hi is calculated with equation B.19, by replacing , p by pi in the calculation of j and f, and Dm by
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