Spherical silica
There are two types of silica gel employed in chromatography either as a stationary phase per se or for the production of bonded phases. The two forms are irregular silica and spherical silica. Irregular silica packing is obtained by grinding and grading amorphous silica to the required particle size. Spherical silica can be prepared by two basic methods. It can be prepared by spraying a neutralized silicate solution (a colloidal silica sol) into fine droplets before gelling has taken place and subsequently drying the droplets in a stream of hot air. The second method is to disperse a silica sol in the form of an emulsion (containing spherical droplets of silica sol) in an appropriate organic solvent and allowing the silica sol to gel (sometimes catalytically promoted by hydrochloric acid or some other catalyst). Spherical silica particles are claimed to give better columns than irregular silica particles but this will depnd very much on the packing procedure employed.
Author: RPW Scott
Book:Liquid Chromatography
Section:HPLC Stationary-Phases Silica-Gel Spherical
The Preparation of Spherical Silica Gel
Spherical
particles of silica can be prepared by spraying a neutralized silicate solution
(the colloidal silica sol.) into fine droplets before gelling has taken place
and subsequently drying the droplets in a stream of hot air. It has also been
shown possible to disperse a silica sol in the form of an emulsion in a suitable
organic solvent where the droplets gel in spherical form (12). Unfortunately,
details for the preparation of spherical silica have tended to be kept very
confidential for commercial reasons and so information is a little sparse. One
of the first methods reported was that of Le Page et al (13,14). A
stable silica sol. (generated at low pH so that gelling does not take place) is
passed through a non aqueous solvent in such a manner as to produce
HPLC Stationary-Phases Silica-Gel Spherical
Author: RPW Scott
Book:The Mechanism of Chromatographic Retention
Section:Retention Exclusion Silica-Gel-Preparation
covers the molecular size of most of the solutes separated on LC columns. It
follows, that silica gel will act as an exclusion media and be capable of
separating substances on the basis of molecular size. The smaller molecules
will enter the majority of the pores and thus, be retained the most. The larger
molecules may be excluded from all the pores and, consequently, will be
retained the least.
Contemporary
silica gel particles that are used per se or for the production of
bonded phases are spherical in shape and made differently. However, the
chemical process of gel formation is very similar and leads to the same porous
material of high surface area with very similar physical properties. Spherical particles of silica can be
prepared by spraying a neutralized silicate solution (the colloidal silica sol)
into fine droplets before gelling has taken place and subsequently drying the
droplets in a stream of hot air. It is also possible to disperse a silica sol
in the form of an
Retention Exclusion Silica-Gel-Preparation
Author: RPW Scott
Book:Liquid Chromatography
Section:HPLC Stationary-Phases Silica-Gel Irregular
a firm, almost rigid gel is produced which is called the hydrogel.
The compact hydrogel is then well washed under controlled conditions to
eliminate the last of the sodium chloride and then heated for a few hours at
120oC. The resulting product is a hard amorphous mass called the xerogel.
The xerogel, ground and graded is the material that is used for packing LC
columns and manufacturing bonded phases. The product, prepared in this way, is
called irregular silica gel, to differentiate it from spherical
silica gel which is prepared by employing an entirely different synthetic
procedure. Irregular silica gel is also the basic material from which bonded
phases can be prepared
HPLC Stationary-Phases Silica-Gel Irregular
Author: RPW Scott
Book:Gas Chromatography
Section:YES GC-Columns Packed-GC-Column Adsorbents
activated form, is used to separate the permanent gases and hydrocarbons up to
about pentane. Alumina is usually activated by heating to 200˚C for about
an hour. A common particle size is about 100/120 mesh and the pore size range
from about 1 Å to 100,000Å. Silica gel in spherical form (prepared by spraying
a neutralized silicate solution (a colloidal silica sol) into fine droplets,
allowing the silica gel to be formed, and subsequently drying the droplets in a
stream of hot air). Silica is produced with a wide choice of surface areas and
porosity's, which can range from about 750 m2/g
and a mean pore size of 22 Å, to a material having a surface area of only 100m2/g and a mean pore diameter of 300 Å. It
is used for the separation of the lower molecular weight gases and some of the
smaller hydrocarbons. In a specially prepared form, silica can be used for the separation
of the sulfur gases, hydrogen sulfide, sulfur dioxide and carbon disulfide.
Molecular
sieves
YES GC-Columns Packed-GC-Column Adsorbents
Author: RPW Scott
Book:Extra Column Dispersion
Section:EC-Dispersion High-Efficiency-GC-Columns
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Employing
equation (1) the volume standard deviation for three popular, contemporary, LC
columns eluting solutes of different (k') values can be calculated. The type of
packing need not be defined and may be silica, bonded silica or polymeric in
character, but all will be assumed to be spherical in form. In fact, the
particle diameter of the stationary phase controls the magnitude of column
dispersion and not its chemical character. A value of 0.6 is taken for (e) which is generally accepted (2). The
properties of the three columns are shown in table 1 including the peak
volume, (4sv), which has more significance to the
practicing chromatographer
It is seen
that the dead volume peak widths are very narrow (assessed as (4sv(k'=0))
and range from about 5 ml
for the peak
EC-Dispersion High-Efficiency-GC-Columns
Author: RPW Scott
Book:Gas Chromatography - Tandem Techniques
Section:GC-Tandem Infrared-Absorption
This toroidal mirror focuses the portion of incident light onto the reference photocell, providing an output that is proportional to the strength of the incident light. The path of the fluorescent light is largely on the right hand side of the diagram. Fluorescent light from the cell is focused by an ellipsoidal mirror on to a spherical mirror at the top right-hand side of the diagram. This mirror focuses the light onto a grating situated at about center right of the figure. This grating can scan the fluorescent light and provide a fluorescent spectrum. Light from the grating passes to a photoelectric cell which monitors its intensity. The instrument is quite complex and, as a result, rather expensive; however, from the point of view of measuring fluorescence it is extremely versatile. Again the cell and all conduits
GC-Tandem Infrared-Absorption