Shodex IC SI-90 4E User manual

ver.211013E
SHOWA DENKO K.K. (https://www.shodex.com/)
1
Operation Manual
Shodex

IC SI-90 4E
（Please read this manual carefully to achieve the best and consistent column performance for a long time）
Important Handling Instructions
Caution! · Please consult the Safety Data Sheet (SDS) of reagents and solvents used with the column
and understand their proper handling methods to prevent potential health hazards or death
from occurring.
· Please wear appropriate personal protective equipment such as lab goggles and gloves
when handling organic solvents and acid and alkaline reagents. Avoid any direct physical
contact to prevent chemical injuries.
Before Using the Column
(1) Please visually inspect the package and outside of the column for any damage.
(2) Please check if product name and serial number written on the column package, column name tag, and
enclosed Certificate of Analysis (CoA) are matching and correct.
1. Introduction
Thank you for purchasing the Shodexproduct. ShodexIC SI-90 4E is a suppressor type ion chromatography
column for analysis of anions, using sodium carbonate eluents. The column is suitable for the separations of
standard inorganic anions including fluoride, chloride, nitrite, bromide, nitrate, phosphate, and sulfate, as well
as organic acid anions such as acetate and formic acid.
2. Column Components
3. Column Specifications
Product
Code Product Name Column Size (mm) Particle Size
(μm)
Theoretical Plate
Number
(Per Column)
I.D. Length
F6995244 IC SI-90 4E 4.0 250 9 ≥5,000
F6709620 IC SI-90G 4.6 10 9 (Guard Column)
Base Material : Spherical porous particles of polyvinyl alcohol modified with quaternary ammonium group
Column Housing : PEEK
Screw Type : Internally-threaded type No.10-32 UNF
Shipping Solvent : 1.8 mM Sodium Carbonate Solution + 1.7 mM Sodium Bicarbonate Solution

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4. Usable Conditions
Usable solvents are listed below.
(1) In general, a mixture of sodium carbonate solution and sodium bicarbonate solution is used.
(2) The standard eluent is 1.8 mM sodium carbonate solution and 1.7 mM sodium bicarbonate solution.
The higher the concentration of sodium carbonate solution, the faster the elution of ions will be.
(3) In case injecting more than 50 μL sample and nitrate and sulfate peaks become broad, or when analyzing a
sample with analytes’ (standard anions) concentrations less than 1 mg/L, use a mixture of 1.0 mM sodium
carbonate solution and 4.0 mM sodium bicarbonate solution.
(4) To simultaneously analyze organic acid anions, such as acetate and formic acid, and inorganic anions, use
12 mM sodium bicarbonate solution.
(5) Up to 10 % (v/v) acetonitrile or methanol is usable.
Attention! · Use the column within above stated flow rate, pressure, and temperature ranges. Using
the column outside the given range may damage the column and lower its performance.
·Column pressure is influenced by the eluent composition, flow rate, and column
temperature. When changing the eluent compositions, adjust the flow rate and column
temperature so that the column pressure remains below the usable maximum pressure.
5. Eluent Preparation
(1) Degas the eluent fully to prevent the formation of air bubbles.
(2) Presence of small debris or insoluble substances may result in deterioration of the column and/or they appear
as noise on the chromatograms. Filter the eluent with a 0.45-μm disposable filter to prevent the problems.
Attention! · Whenever water is required, use ultra-pure water freshly generated by a water purification
system or water from a newly opened HPLC grade distilled water bottle. Use HPLC grade
organic solvent whenever possible. Solvents left in an opened bottle for a long time should
not be used. The content may have been changed, absorbed moisture, or has been
contaminated.
· Always use freshly prepared solvents. Solvents stored for a long time may have changed
their compositions and may influence elution patterns and/or damage the column.
Note · Use of on-line degasser is recommended.
6. Sample Preparation
(1) Filter the sample solution using disposable 0.45-μm filter to prevent the column from clogging or deteriorating.
(2) Recommended sample injection volume is less than 50 μL per column.
(3) For the samples containing proteins, remove the proteins prior to the sample injection. The use of an
ultrafiltration membrane is recommended.
(4) For the samples containing hydrophobic impurities, remove the impurities prior to the sample injection. The
use of a solid phase extraction is recommended.
Note · Use of guard column is recommended to protect the analytical column.
Product Name Flow Rate (mL/min) Maximum
Pressure (MPa)
(Per Column)
pH
Range
Temperature (°C)
Recommended Maximum Recommended Range
IC SI-90 4E 1.0 2.0 10 3 - 12 25 20 - 60
IC SI-90G - - -

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7. Column Usage Procedure
7.1 HPLC System Preparation
Wash entire LC system prior to the column installation, including all flow-lines and sample loop by switching the
valve, and then replace the washing solution with the eluent to be used. If desired new eluent has low
miscibility/solubility to the eluent of previous analysis, first use the eluent that is miscible/soluble to both eluents,
and then replace it with the desired eluent.
Attention! · If the eluent left in the system is not compatible with the column to be used, it may damage
the column.
· A drastic change in the eluent compositions may remove substances adsorbed on the
system and they may enter and deteriorate the column.
7.2 Column Installation
(1) Connect the column to LC system by following the “flow direction arrow” (➡) indicated on the column name
tag. If guard column is used, position the guard column in front (before the inlet) of the analytical column.
(2) Make sure to insert the tubing all the way to the end fitting and secure it with the male nut. It is important that
there is no extra space between the tubing and the column side of the end fitting. Presence of an extra space
will let the sample to spread out and may result in wide peaks.
(3) Set the initial flow rate at less than 0.5 mL/min and start the system. If using the column at an elevated
temperature, keep a low flow rate until the temperature of the column reaches to the set temperature, and
then gradually increase the flow rate to the desired.
Caution! · Verify that there is no solvent leak. It may cause electronic leakage, rust, and/or chemical
injury.
Attention! · Make sure not to let air bubbles enter the column while installing the column. The air
bubbles may damage the column.
· When restarting the system after column installation or after holding the eluent flow, start
the system at less than 0.5 mL/min. A rapid increase in pressure can damage the column.
· If the column was used at an elevated temperature, lower the flow rate to less than
0.5 mL/min at the end of analysis. Then, turn off the column oven, and let the column
temperature return to room temperature before stopping the pump. If the pump was
stopped while the eluent inside the column was still hot, as the eluent temperature
decreases, its volume also decreases. This may result in creating an empty space in the
column and deteriorates the column.
Note · It is recommended to set the pump limiter to avoid exceeding the maximum pressure.
7.3 Solvent Exchange
When replacing the solvent, start the system at less than 0.5 mL/min. Recommended solvent volume to
introduce at each step is 3 to 5 times of the column volume.

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7.4 Column Cleaning
Problems in peak shapes and elution time changes or elevated column pressure etc. are often caused by
insoluble or adsorbing components present in the eluent and reagents being deposited inside the column. These
problems may be resolved by cleaning the column.
If a guard column is used with the analytical column, first remove the guard column and check the performance
of the analytical column alone. If the problem is solved, most likely the cause is from the guard column. In this
case, clean the guard column.
If the problem is not solved by removing the guard column, clean both guard and analytical columns. Make sure
to clean the guard and the analytical columns separately. When washing the column, let the washing solution
flow from the column outlet go directly into the waste container and not let the solution go through the detector.
<Cleaning Method>
(1) Insoluble components that block the column inlet may be removed by reversing the flow direction, i.e.,
introducing the eluent from the column outlet, with flow rate at less than half of the recommended flow rate.
(2) Follow below cleaning steps for adsorbing components. For an efficient cleaning, reverse the flow direction
and use the flow rate at 0.5 mL/min.
Method 1: Adsorption of hydrophilic compounds
Washing Solution Cleaning Time
1 H2O 15 min
2 10 x Concentrated Eluent 60 min
3 H2O 15 min
4 Eluent (Return the column flow to normal direction) 60 min
Method 2: Adsorption of hydrophobic compounds
Washing Solution Cleaning Time
1 H2O 15 min
2 H2O/CH3CN = 95/5 10 min
3 CH3CN 60 min
4 H2O 30 min
5 Eluent (Return the column flow to normal direction) 60 min
Method 3: When abnormal nitrate peak (tailing, unsymmetrical etc.) was observed.
Note: Keep the normal column flow direction.
Washing Solution Cleaning Time
1 H2O 15 min
2 1 M Sodium Carbonate Solution 25 min
3 *Remove the column from the system, tighten the end caps, and store
the column at room temperature for 3 days.
4 Eluent 60 min
*Leaving it for more than 4 days can damage the column.
Attention! · Leaving the washing solution in the column for an extended time can damage the column.
Do not suspend the column cleaning, but complete all procedures until the last step to
replace it with the eluent.
8. Column Storage
Remove the column from the system after replacing the in-column solvent with the shipping solvent. Securely
tighten the end caps and store the column at a location with stable temperature (a cool and dark space is
recommended). Refer to section 7.3 Solvent Exchange for how to replace the eluent.
Attention! · Never allow inside of the column to dry. It can damage the column.

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9. Column Inspection
Inspection method is described in the Certificate of Analysis (CoA).
Theoretical Plate Number (N) and Asymmetry Factor (Fas) were calculated using the below equations.
(1) Theoretical Plate Number (N)
(2) Asymmetry Factor (Fas)
10. Additional Warnings
(1) Do not remove end fittings.
(2) Do not make a strong impact on the column. Do not drop or hit the column on a hard surface.
Refer to the Shodex™ website (https://www.shodex.com/) for product details and their applications.
For additional assistance, contact the distributor from whom you purchased the column or contact your regional
Shodexsupport office (https://www.shodex.com/en/support_office/list/).