UNISIL Technical Data
Unisil is a specifically prepared silica acid that has been processed
to an exceptional degree of uniformity in order to provide maximum resolution
of closely related organic materials. Quality control of three factors
has been maintained in preparing this silicic acid. The product has been
thoroughly acid- washed to remove trace mineral impurities that might
provide sites for irreversible absorption of some substances. In addition,
"tailing" phenomena are minimized by the use of acid-washed silicic acid.
Finally, the particle size of Unisil has been controlled, by sieving,
to a narrow range. The grades we offer -100-200 mesh, 200-325 mesh - are
completely free of dust. Consequently, flow rates of common eluting agents
such as hexane, chloroform, benzene, ethyl acetate and methanol are such
that the use of diatomaceous earth as a diluent is not necessary. With
small scale columns, using 10-20 grams of absorbent, flow rates of 2-6
m./min are easily obtained, while colums containing a pound of silicic
acid have given flow rates up to 20 ml/min.
Unisil offers complete fractionation in one column with a relatively
small quantity of silicic acid. Duplication of separations is very good.
It is an excellent material for separation of lipids such as neutral
non-glyceride lipids, glyceride lipids, glycolipids, phospholipids,
cholesterol, and the like.
The moisture content of silicis acid is often an important factor
controlling separations-especially with the use of non-polar solvents
as eluting agents. Unisil is supplied in a heat-activated form by drying
at 100 degrees centigrade for 12-15 hours just prior to shipping. This
treatment provides a medium moisture content that is optimum for many
separations.
A standard procedure for refining silicic acide is: A preliminary
screening is carried out by dry sieving, and all material passing a
325-mesh screen is discarded. Approximately 100 grams of silicic acid
is treated with 250 ml of 3 N hydrochloric acid in a glass vessel and
stirred for 30 minutes with a nonmetallic pa ddle. This silicic acid
is allowd to settle, the aqueous acid decanted, and the residue washed
repeatedkt with deionized water for two days until the supernatant liquid
reaches a pH of 4.5 ti 5.5. Usually 20 to 40 water changes are required.
The silicic acid is then washed with acetone, filtered, resuspended
several times in fresh acetone, then dried in glass trays under an infrared
lamp for 16-20 hours. A final screening provides material of 100-to
200 mesh size, which is dried in an oven with 20 to 25 inches vacuum
for two hours at 50 degrees centigrade. It may be kept in closed containers
for several months without apparent change. Used silicic acid is washed
with methanol, followed by deionized water an acetone, and dried as
in the original preparation.
At Clarkson we've modified this standard procedure to produce the
highest grade silicic acid available.
Laboratory Analysis
Unisil
Activated Silicic Acid
100-200 Mesh and 200-325 Mesh
Maximum Limits |
Loss on Ignition |
8.000% |
Loss on Drying |
Min. 5.000% |
Chlorine (Cl) |
.010% |
Heavy Metals (Pb, for example) |
.002% |
Iron (Fe) |
.001% |
Nonvolatile with HF |
.200% |
Organic Impurities |
.001% |
Chromatography Grade Silicic Acid
100-200 Mesh and 200-325 Mesh, and Powder
Maximum Limits |
Loss on Ignition |
10.000% |
Loss on Drying |
Min. 5.000% |
Chlorine (Cl) |
.010% |
Heavy Metals (Pb, for example) |
.002% |
Iron (Fe) |
.001% |
Nonvolatile with HF |
.200% |
Availability
Clarkson UNISIL is available in 100-200 Mesh, 200-325 Mesh in
100 gram bottles or by the case (six 100 gram bottles to a case).
Chromatography grade Silicic Acid is available in 100 Mesh, and through
325 Mesh and is packaged in 500 gram bottles and 100 lb. drums. (Price
reduction for multiple drum orders.)
Material Handling
Silicic acid can range in PH from 4.5 to 7.0. It is water loving and midly
corrosive. Silica dust mask and gloves must be worn when handling the
powder on a regular basis.
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