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• 11 •
www.restekcorp.comBulk HPLC Silica and Bonded Phase Packings
For Scale-Up or Other Applications
By Greg France, HPLC Product Marketing Manager
✔
Consistent, high-quality porous spherical silicas for
• neutral to slightly acidic compounds
• basic compounds.
✔
Silica and bonded materials rigorously tested; ISO 9001:2000 registered facility.
Restek is one of the few HPLC column suppliers
manufacturing chromatography grade silica. We now
offer our high-quality silicas and bonded phase
materials in bulk, for packing analytical-scale
columns, for preparative and process purification, or
as raw materials for other LC analytical platforms.
Pinnacle II
™
is a Type A spherical silica with a mean
pore size of 110Å and a surface area of 180m2/g. It
matches Hypersil
®
silica in many respects, but the
metals content in Pinnacle II
™
is almost an order of
magnitude less than that in Hypersil
®
silica.
1
Practically, this is expressed as a less active surface
and a more durable particle. Packings based on
Pinnacle II
™
silica are excellent for analyzing or
purifying neutral to slightly acidic compounds
(Figure 1). Standard particle sizes for Pinnacle II
™
materials are 3µm and 5µm; 10µm and 15µm parti-
cles are available on request.
Highly base-deactivated Pinnacle
™
DB silica has
mechanical strength and durability similar to
Pinnacle II
™
silica, but Pinnacle
™
DB silica has larg-
er pores (140 Å). The total metals content is less
than 250ppm, and no single metal exceeds
100ppm.
2
Packings based on Pinnacle
™
DB silica are
suitable for a wide range of analytes; basic analytes
often can be analyzed with little or no mobile phase
Metal ions on a silica particle weaken the particle
and negatively affect chromatography, particularly for
basic analytes. These problems can be overcome—
temporarily—by annealing the metals into the
framework of the particles. As the particles age, the
metals are re-exposed. Base deactivation is lost and
the particles' stability in highly aqueous mobile phas-
es is further eroded.
Pinnacle II
™
and Pinnacle
™
DB silicas do not require
annealing; they provide more consistent peak shapes
for bases as the column ages, and a potentially
longer column lifetime.
Figure 1
—Morphine sulfate resolved from manufacturing solvent,
using a Pinnacle
II
™ C18 column (USP 25 Resolution Solution).
Figure 2
—Sharp, near-symmetric peak for a
basic analyte (pyridine) without a mobile phase
modifier, using a Pinnacle™ DB column.
modifier (Figure 2). Performance is very similar to
Hypersil
®
BDS material.
Our extensive QC program ensures the quality and
reproducibility of Pinnacle II
™
and Pinnacle
™
DB sil-
icas: each lot of material must meet specifications
for mean particle size, particle size distribution, pore
diameter, surface area, and total metals content. You
can use these materials with confidence.
Column:
Pinnacle
II
™
C18
Cat.#:
9214575-700
Dimensions:
250 x 4.6mm
Particle Size:
5µm
Pore Size:
110Å
Conditions:
Mobile Phase:
A: 0.73g 1-heptane sulfonic acid and 10mL glacial acetic
acid diluted to 720mL with water, pH=2.33
B: methanol
72A:28B, v/v
Flow:
1.00mL/min
Temp.:
26.5°C
Det.:
UV @ 284nm
Sample:
Inj.:
20.0µL
Solvent:
mobile phase
LC_0209
Peak List:
Conc.
(µg/mL)
U. unknown
unknown
1. phenol
0.15
2. morphine sulfate 0.24
Column:
Pinnacle
™
DB C18
Cat. #:
9414565
Dimensions:
150 x 4.6mm
Particle Size:
5µm
Pore Size:
140Å
Conditions:
Mobile Phase:
water:methanol (40:60 v/v)
Flow:
1.0mL/min.
Temp.:
ambient
Det.:
UV @ 254nm
Sample:
Inj.:
5µL
Sample Diluent:
methanol:water (50:50 v/v)
0
2
4
6
1
2
3
4
8
10
min.
LC_0276
3µm Pinnacle
II
™ Bulk Packing Materials
Description
min. qty.
cat.#
price per gram
Pinnacle
II
™
C8 Bulk Packing
5g
92133
Pinnacle
II
™
C18 Bulk Packing
5g
92143
Pinnacle
II
™
Cyano Bulk Packing
5g
92163
Pinnacle
II
™
Phenyl Bulk Packing
5g
92153
Pinnacle
II
™
Silica Bulk Packing
5g
92103
5µm Pinnacle
II
™ Bulk Packing Materials
Description
min. qty.
cat.#
price per gram
Pinnacle
II
™
C8 Bulk Packing
5g
92135
Pinnacle
II
™
C18 Bulk Packing
5g
92145
Pinnacle
II
™
Cyano Bulk Packing
5g
92165
Pinnacle
II
™
Phenyl Bulk Packing
5g
92155
Pinnacle
II
™
Silica Bulk Packing
5g
92105
5µm Pinnacle™ DB Bulk Packing Materials
Description
min. qty.
cat.#
price per gram
Pinnacle
™
DB C18 Bulk Packing
5g
94145
Pinnacle
™
DB C8 Bulk Packing
5g
94135
Pinnacle
™
DB Cyano Bulk Packing
5g
94165
Pinnacle
™
DB Silica Bulk Packing
5g
94105
1
Request publication 59517.
2
Request Applications Note 59742.
Peak List:
Conc.
1. uracil
1.0µg/mL
2. pyridine
0.64mg/mL
3. N,N-dimethylaniline
0.45mg/mL
4. benzophenone
0.59mg/mL
Tech
Tip
!
HOT
How important is metals content?
1
2
U