Shodex RSpak KC-811 User manual

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
Operation Manual
Shodex™ RSpak™ KC-811 and KC-811 6E
Europe, Middle East, Africa, Russia
www.shodex.de
Sales Office:
Showa Denko Europe GmbH
Shodex Business
Konrad-Zuse-Platz 3
81829 Munich
Germany
Technical Support:
[email protected]
+49 (0)89 / 93 99 62 37
Quotes and Orders:
[email protected]
+49 (0)89 / 93 99 62 34

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
2
Operation Manual
Shodex™ RSpak KC-811 and KC-811 6E
(Thank you for purchasing a Shodex product. Prior to use, be sure to read this instruction manual so
that the maximum service life and performance can be achieved.)
1. Introduction
Designed for chromatography by a combination of ion exclusion and partition/adsorption, the Shodex
RSpak KC-811 column is packed with ion-exchange resin gels of sulfonated rigid styrene-divinylbenzene
copolymer and demonstrates an excelling performance in separating low-molecular weight organic
acids and water-soluble organics such as alcohols, aldehydes and nitriles. Shodex RSpak KC-811 6E is
suitable for analyzing cyanide (CN) ion and cyanogen chloride (CNCl). Combination of ion
chromatograph and postcolumn absorptiometric method is applied to this analysis.
2. Handling Instructions
Caution! Take notice of keeping instructions about the solvents and the reagents used with the column
not to occur problems related to losing your health or leaking.
Attention! Use the column within the regular range of flow rate, pressure and temperature. There is a
danger of deteriorating the performance when it is handled beyond the permissible range even for a
short time. See the Section 4. Usable Conditions for the permissible ranges.
3. Specifications
Product code
Product name
Functional
group
Size (mm)
Particle size
(μm)
Plate Number
(per column)
ID
Length
F6378030
RSpak KC-811
Sulfo
8.0
300
6
≥ 17,000
F6378033
RSpak KC-811 6E
Sulfo
6.0
250
6
≥ 13,000
F6700010
RSpak KC-G 8B
Sulfo
8.0
50
13
(Guard column)
F6700030
RSpak KC-G 6B
Sulfo
6.0
50
10
(Guard column)
Packing material: Styrene divinylbenzene copolymer
Functional group: Strong cation-exchange resin gel with Sulfo-groups
Column material: Stainless steel SUS-316
Screw type: Unified Thread Standard No. 10-32 UNF
Shipping solvent: 0.1% phosphoric acid (H3PO4) aqueous solution
Use RSpak KC-G 8B for samples with relatively high impurity.
Use RSpak KC-G 6B for samples with relatively low impurity.
4. Usable Conditions
Product name
Max. flow rate
(mL/min)
Max. pressure
(MPa)
Max. organic
solvent
Working temperature
range (°C)
RSpak KC-811
1.5
5
20%
40-85
RSpak KC-811 6E
1.0
2.5

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
3
5. Mobile Phase
1) An aqueous solution containing 0.1% phosphoric (H3PO4) or perchloric acid (HClO4) is normally used
as the mobile phase. Also sulfuric acid (H2SO4) aqueous solution could be used. Concentration of the
acid is around 1-6 mM.
Caution! Do not use hydrochloric acid aqueous solution as the mobile phase since it corrodes the
column.
2) Remove extraneous substances and insolubles from the mobile phase by passing it through a
0.45 µm filter into a bottle and thoroughly degas it by, for instance, heating to about 60°C in a hot
water bath and shaking in an ultrasonic washing vessel, with the ambient air pressure being
simultaneously reduce by an aspirator. Use of solvent degassing device will facilitate the degassing
work.
Note! Molecules of highly hydrophobic specimens are too slow to flow out of the column due to their
adsorption onto the packing. In such a case, add ethanol in an amount up to 20% to the mobile phase
to reduce the absorptivity.
6. Mounting and Start-up
1) Before mounting the column on the liquid chromatograph, replace thesolvent in the chromatograph
with the mobile phase.
Caution! In replacing a water-insoluble organic solvent in the chromatograph, replace it first with a
water-soluble organic solvent, such as acetone or ethanol, and then replace the water-soluble solvent
with the mobile phase.
2) Set the flow rate at 1/0.5 mL/min.
3) Connect the column to the chromatograph in such a way that the arrow mark on the column will
point to the flow direction.
Caution! Do not let the air into the column during the connection.
4) Heat the column to 40-50°C and start the pump.
Caution!
i) Keep the column pressure below 5/2.5 MPa per column; otherwise, the column will be ruined.
ii) The Maximum working flow rate depends on the working temperature, as follows:
Working temperature (°C)
Maximum working flow rate
RSpak KC-811
RSpak KC-811 6E
40 –85
1.5 mL/min
1.0 mL/min
30 –39
1.0 mL/min
0.5 mL/min
29 or below
0.5 mL/min
0.2 mL/min
iii) Do not abruptly change the column pressure or flow rate.
iv) Do not heat the column higher than 85°C.

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
4
7. Pre-treatment of Specimen
1) When the specimen is solid, dissolve it, using some of the degassed mobile phase.
Note: Do not use any other solvent; otherwise, the solute sometimes settles in the mobile phase to
plug the column.
2) When the specimen is liquid and contains an organic solvent such asalcohol, dilute it with themobile
phase so as to reduce concentration of the organic solvent to 20% maximum; otherwise, the column
performance will deteriorate.
3) Pass the specimen through a 0.45 µm filter to remove extraneous substances and insolubles. Use of
the disposable filter unit is recommended.
4) When the specimen contains proteins, add 2 or 3 drops of distilled water in which sulfosalicylic acid
is dissolved at the rate of 20 g/dL, to 5 mL of the specimen, stir and pass it through a 0.45 µm filter to
remove the proteins.
8. Dismounting and Storage
1) Set the flow rate at 0.2 mL/min, turn off the heater and let the column stand as is until it cools down
to room temperature.
2) Stop the pump and dismount the column.
3) Cap both ends of the column, put it back in the same case in which it was delivered from the
manufacturer, and store the case in a place where the temperature does not fluctuate more than ±5°C.
Caution!
i) Do not remove the end fittings of the column; otherwise, its performance will deteriorate or the
column may become unserviceable.
ii) Do not let the in-column solvent freeze during storage; otherwise, the column will swell and become
unserviceable.
iii) Storage at abnormally high temperatures will also cause the swelling to render the column
unserviceable.
9. Guard Column
It is recommended that Guard column RSpak KC-G be installed immediately upstream of the column
to protect the packing from contamination by dirt or readily adsorbable substances in the specimen,
such as metal ions and amino compounds. Use KC-G 8B for samples with relatively high impurity and
KC-G 6B for samples with relatively low impurity.

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
5
10. Performance Test
The column performance can be checked by calculating the number of theoretical plates under the
following conditions:
1) Specimen 3% Acetic acid
2) Injection amount 5 µL
3) Mobile phase 0.1% Phosphoric acid aqueous solution
4) Flow rate 1 mL/min
5) Column temperature 40°C
6) Detector High-sensitivity refractive index detector such as Shodex RI
7) Calculation formula NTP = 5.54 x (Rt/W)2
where NTP: Number of theoretical plate, Rt: Retention time, W: Peak half width
11. Attention
1) Do not remove the end fittings of the column under any circumstances.
2) Do not make a strong impact on the column: such as hitting or dropping on the floor.
3) Replace the solvent in the LC system with the eluent to be used before connecting the column.
4) Connect the column so that the flow direction corresponds to the arrow mark on the tag.
5) When the column is not used for a month or more, replace the in-column solvent with the shipping
solvent, remove it from the LC system, close each end with a stopper, and store it at controlled room
temperature.
6) Filtrate the sample witha disposable filter (0 .45 µm) to prevent deterioration by adsorbing insoluble
matters.
7) Contact Shodex website (www.shodex.de) or Shodex partners regarding product and analysis
applications.

Operation Manual Shodex RSpak KC-811 and KC-811 6E Version 2020
6
12. Warranty (Version 3)
1) Showa Denko K.K. warrants that the ShodexTM Column, at the time of delivery to the user, will
conform to the specification of the attached Certificate of Analysis, if the Shodex Column is used in
accordance with the attached operating manual. The foregoing warranty is exclusive and is in lieu of
all other warranties with respect to the Shodex Column, whether written, oral, implied, statutory or
otherwise. No warranties by Showa Denko K.K. are implied or otherwise created, including, but not
limited to, the warranty of merchantability and fitness for particular purposes.
2) Any claim of inconformity to the specification must be notified to Showa Denko K.K. within ten (10)
days after delivery to the user. User’s exclusive remedy and Showa Denko K.K.‘s exclusive liability for
such claim are limited to the replacement of the Shodex Column in question. In no event is Showa
Denko K.K. liable for any indirect, incidental or consequential damage arising out of in connection with
the Shodex Column, whether or not such damage is allegedly based on breach of warranty, negligence
or otherwise.
3) No warranty is made in any of the following cases:
3-1) If the Shodex Column is not used in accordance with the operating manual
3-2) If the Shodex Column is remodelled by anyone other than person or firm designated by
Showa Denko K.K.
3-3) If the Shodex Column is disposed of
3-4) If the Shodex Column is resold by the user without giving prior written notice to Showa
Denko K.K.
3-5) If the performance of the Shodex Column is not conform to the specification of the
attached Certificate of Analysis due to any of the reasons below:
a) Computer virus
b) Impurities contained in the sample, reagent, gas air or cooling water provided by
the user
c) Breakdown or malfunction of equipment, apparatus or component used in
combination with the Shodex Column
d) Force majeure such as fire, earthquake, flood, other natural disaster, crime, riot, act
of terrorism, war or radioactive contamination
4) In no event is Showa Denko K.K. liable for
4-1) the results of analyses or preparations using the Shodex Column or any portion of the
same, including, but not limited to, the reliability, accuracy, efficacy and safety of said results,
and
4-2) the occupational hazard in the use of the Shodex Column, whether or not such use is made
in accordance with the attached Conditions for use.
5) The Shodex Column is for laboratory use only. It must not be used for clinical diagnosis. Showa
Denko K.K. is not liable for any use of the Shodex Column except laboratory use.