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  9. Shimadzu Shim-pack GIST Series User manual

Shimadzu Shim-pack GIST Series User manual

ERAD-0001-9007
High Performance Packed Column for HPLC
GIST/GISS Series
Shim-pack
INSTRUCTION MANUAL
Introduction
To maintain and maximize peak performance of Shim-pack
GIST/GISS series columns, and to ensure the long life and stability
of columns, please read the following instructions before use.
Specifications
The product specifications of Shim-pack GIST/GISS series
columns are as follows.
Operating Precautions
Check if anything is missing or damaged. If there are any signs of
damage, notify your local Shimadzu representative at once.
Each of the Shim-pack GIST/GISS series columns is delivered with
a Column Performance Report. The information supplied in the
report include the lot number, column serial number, and
chromatographic test conditions. Please keep the report for future
reference.
Column Performance
Shim-pack GIST/GISS series packing materials are subjected to a
rigorous array of QC tests, with special emphasis on reagent purity,
raw material traceability, consistency in raw materials, and quality
of final products. A detailed analysis of all of the physical and
chemical properties of these columns, combined with tests for
chromatographic selectivity and column packing material efficiency,
ensure that each lot of these columns are identical to all previous
lots and column-to-column reproducibility is of the highest order.
Shim-pack GIST/GISS series columns are shipped with the solvent
used for the final QC test of the column, as detailed in the Column
Performance Report delivered with the column.
In the case of NH2 columns, when switching between solvents with
significantly different polarities, first purge the column with a
mutually miscible solvent such as Isopropyl alcohol at a reduced
flow rate (approximately 50% lower than the normal flow rate).
Flush the column with the solvent five times more than the column
volume (e.g. 10 mL for a 150 mm x 4.6 mm I.D. column).
Column Installation
The flow direction of the column is shown on the column (→).
When installing the column, ensure that the flow direction matches
the mobile phase flow direction.
Use PEEK tubing (UHPLC: SUS tubing) with an inner diameter of
0.25 - 0.3 mm (UHPLC: 0.1 - 0.2 mm) and an outer diameter of 1.6
mm.
Use the shortest possible tubing connection from the injector to the
column to minimize peak broadening.
The column should be connected with male nuts. Ensure that the
fittings are connected properly to avoid creating dead volume
between the tubing and the column interface. Male nuts can be
ordered by referring to the part number below.
If peaks are tailing more on the early eluting compounds than later
eluting compounds, there is a possibility that there is a dead volume.
In such case, check that all column connections are properly
connected.
Also, make sure to use appropriate internal diameter and length size
of tubing at the injector and detector, especially when using semi-
micro size columns, to avoid system dead volumes.
Sample
Samples should be dissolved in an eluent or solvent weaker than the
mobile phase, which helps avoid sample precipitation at column
inlet/head and inconsistent retention values.
Clogging of column
The most common cause of the increase of column back pressure or
split peaks is blockage of the inlet filter by sample particulates,
particles created by aging pump seals, or large quantities of
lipophilic compounds adsorbing to the head of the column.
•Filtrate the mobile phase using a 0.45 μm membrane filter before
using the column.
•Installing “Ghost Trap DS” between the pump and injector can
efficiently remove particulates or contaminants in the mobile
phase.
Item name P/N Remarks Pressure
Male nut, PEEK 228-18565-84 5 pcs 20 MPa
Male nut 1.6 MN 228-16001 1 pc 130 MPa
Ferrule 1.6 F 228-16000-10 1 pc 130 MPa
UHPLC Fitting 2 S 228-56867-41 1 pc 130 MPa
Type Columns Stationary Phase Base
Material
Reversed-
Phase
Shim-pack GIST C18
Shim-pack GIST C18-AQ
Shim-pack GISS C18
Octadecyl Groups
(C18)
High purity
porous
spherical
silica
Shim-pack GIST C8 Octyl Groups (C8)
Shim-pack GIST Phenyl Phenyl Groups
Shim-pack GIST Phenyl-
Hexyl
Phenyl-Hexyl
Groups
Normal-
Phase Shim-pack GIST NH2 Aminopropyl Groups
NOTE Stains or air in the flow line may deteriorate the column. Before
connecting the column, be sure to flow the mobile phase to flush
the flow line.
•Filtrate the sample using a syringe filter before injecting to the
column.
•Installing “Guard Column” or “Guard Column for UHPLC” can
prevent column clogging problems.
Baseline drift and noise can be caused by defective pumping due to
air bubbles in eluent or decrease of light intensity when using a UV
detector. Note that bubbles can form in the detector flow cell if the
eluent is not degassed properly before introduction into the column.
Column Handling Precautions
Do not drop or bump the columns, to avoid a deterioration of the
column performance.
To maximize column life, use the columns within the pressure
shown in the following table.
Avoid rapid pressure fluctuation.
Column should be disconnected from the system after the pressure
gauge indicates “0”.
Please note that operating the sample injection valve slowly or
using an auto-sampler with slow valve switching speed will also
generate a rapid pressure increase at the column inlet, which will
cause premature column deterioration.
For operating temperature and pH limits, please refer to the
following table.
* The contents of this instruction sheet are subject to change without notice.
Flow rate of Prep column
Please read the following instructions before using prep columns.
•The optimum performance will be gained in the range of flow
rate listed below. Even so, since the column may have
considerable pressure, we recommend you to use the column at
pressure less than 20 Mpa. When using a 100 mm I.D. column,
use the pressure within 10 MPa.
•The flow rate will be larger than that of analytical columns. Use a
0.8 mm or 1.0 mm I.D. tubing accordingly.
•We recommend you to use an injection valve with a bypass to
prevent the column from deterioration.
Storage of Columns
After using reversed-phase columns with eluent containing buffer
or ion-pair reagent, wash the column thoroughly with a salt-free
eluent before storing. When storing the column for a long period,
replace with 100% organic solvent such as methanol.
After using NH2 columns for sugar analysis with reversed-phase
mobile phases, such as acetonitrile/water or buffer salt, first
introduce ammonium formate aqueous solution or ammonium
acetate aqueous solution to flush the column, then flush the column
with HPLC grade water. When storing the column for a long period,
replace with 100% acetonitrile, completely seal the column with the
plugs provided, and store it in a temperature stable place.
After using NH2 columns with normal-phase mobile phases,
introduce ethanol or 2-propanol to flush the column. When storing
the column, replace with n-hexane/2-propanol=90/10, v/v,
completely seal the column with the plugs provided, and store it in
a temperature stable place.
Technical Support
Shim-pack GIST/GISS series columns are manufactured, inspected,
packaged and shipped under strict standards of quality control.
Should you find any defect in performance, please contact your
local Shimadzu representative, who will ensure your complete
satisfaction.
We regret that we cannot guarantee the lifetime of columns, also
that we cannot accept any claim when performance has deteriorated
due to noncompliance with the operation procedures elucidated
above, or as a result of normal aging.
Particle
Size
Column
Dimensions
Recommended Operating Pressure
(Maximum Operating Pressure)
1.9 μm,
2 μm
Column lengths
shorter than 75 mm
Under 50 MPa
(80 MPa)
1.9 μm,
2 μm
Column lengths
longer than 100 mm Under 80 MPa
HP 3 μm All sizes Under 50 MPa
3 μm,
5 μm All sizes Under 20 MPa
Columns pH Range
(From 20-40℃)
Maximum Operating
Temperature
Shim-pack GIST C18
Shim-pack GIST C18-AQ
Shim-pack GISS C18
1-10 *1,2,3 60℃
(pH 1-7)
50℃
(pH 7-10)
Shim-pack GIST C8
Shim-pack GIST Phenyl-
Hexyl
1-10 *1,2,3 60℃
(pH 2-7)
50℃
(pH 7-9)
Shim-pack GIST Phenyl
Shim-pack GIST NH2 2-7.5 60℃
(pH 2-7.5)
NOTE
* 1 If you use the column with eluents at pH1 - pH2 or pH9 - pH10, we
recommend you to keep column temperature lower and use
the eluent contained trifluoroacetic acid, formic acid, acetic acid,
phosphate buffer or organic buffer, such as 5 mM triethylamine. If
you use the column without organic solvent, we suggest you to use
the column within the pH range of pH2 - pH8.
* 2 To maximize the column lifetime, set the pH of the mobile phase
within the range shown in the above table.
* 3 To maximize the column lifetime, lower the column temperature
when the pH of the mobile phase from 1-2 and 9-10. In addition, use
mixed mobile phase such as organic solvent and buffer rather than
100% buffer.
Inner diameter Flow rate range
7.6 mm 2 - 4 mL/min
8.0 mm 2 - 4 mL/min
10 mm 3 - 5 mL/min
14 mm 5 - 10 mL/min
20 mm 10 - 20 mL/min

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