Thermo Scientific IonPac CS16 User manual

Errata
Product Manual for Dionex IonPac™ CS16 and CG16 Columns
031747-05
For new orders of the following parts discussed in this manual, please use the updated part
numbers listed below.
Part Old Part Number in this
manual Updated Part Number to use for new orders
PROD,COL,IP,CS16,5X250MM 057573 079805
PROD,COL,IP,CG16,3X50MM 059595 079931

IonPac®CS16
IonPac®CG16
for

Product Manual for IonPac CS16 Page 1 of 65
Product Manual
for
IONPAC®CG16 GUARD COLUMN
5 x 50 mm, P/N 057574
3 x 50 mm, P/N 059595
0.5 x 50 mm, P/N 075402
IONPAC®CS16 ANALYTICAL COLUMN
5 x 250 mm, P/N 057573
3 x 250 mm, P/N 059596
0.5 x 250 mm, P/N 075401
© 2010 Dionex Corporation
Document No. 031747
Revision 05
December 2010
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 2 of 65
TABLE OF CONTENTS
SECTION 1 – INTRODUCTION............................................................................................................ 4
SECTION 2 – THE ION CHROMATOGRAPHY SYSTEM.............................................................. 6
SECTION 3 – INSTALLATION............................................................................................................. 8
3.1.System Requirements ......................................................................................................................................8
3.1.1.System Requirements for 0.5 mm Operation.....................................................................................................8
3.1.2.System Requirements for 5-mm Operation.......................................................................................................8
3.1.3.System Requirements for 3-mm Operation.......................................................................................................8
3.1.4.Installation of the Capillary Column .................................................................................................................8
3.2.Installing the CR-CTC Trap Column for Use with EGC MSA Cartridge...............................................12
3.3.Installing the Cation Trap Column for Eluent Step Change or Gradient Operation..............................12
3.4.The Injection Loop.........................................................................................................................................13
3.5.Sample Concentration...................................................................................................................................13
3.6.IonPac CG16 Guard Columns......................................................................................................................14
3.7.Eluent Storage................................................................................................................................................14
3.8.Cation Self-Regenerating Suppressor and
Cation Capillary Electrolytic Suppressor Requirements...........................................................................14
3.9.Cation Atlas Electrolytic Suppressor Requirements ..................................................................................14
3.10.Cation MicroMembrane Suppressor Requirements...................................................................................14
3.11.Using Displacement Chemical Regeneration (DCR) with the Chemical Suppression Mode..................14
3.12.Using AutoRegen®with the Chemical Suppression Mode.........................................................................15
3.13.Detector Requirements..................................................................................................................................15
SECTION 4 – OPERATION ................................................................................................................. 16
4.1.General Operating Conditions......................................................................................................................16
4.2.Operating Precautions...................................................................................................................................16
4.3.Chemical Purity Requirements.....................................................................................................................16
4.3.1.Deionized Water..............................................................................................................................................16
4.3.2.Inorganic Chemicals........................................................................................................................................17
4.4.Preparation of Eluent Stock Solution Concentrates...................................................................................17
4.4.1.1.0 N Methanesulfonic Acid (MSA) Stock Solution.......................................................................................17
4.4.2.1.0 N Sulfuric Acid Stock Solution.................................................................................................................17
4.4.3.Eluent Preparation ...........................................................................................................................................18
4.5.Eluents with Solvents.....................................................................................................................................18
4.5.1.Making and Using Eluents that Contain Solvents ...........................................................................................20
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 3 of 65
SECTION 5 – EXAMPLE APPLICATIONS ...................................................................................... 21
5.1.Production Test Chromatogram at 40 °C....................................................................................................22
5.2.Reproducing the Production Test Chromatogram Using a Sulfuric Acid Eluent at 40 °C.....................24
5.3.6-Cations (Li+, Na+, NH4+, K+, Mg2+, Ca2+) with CS16 3-mm and CAES.................................................25
5.4.6-Cation Fast Run (Li+, Na+, NH4+, K+, Mg2+, Ca2+) at 40 °C ....................................................................26
5.5.6-Cation Run (Li+, Na+, NH4+, K+, Mg2+, Ca2+) at Room Temperature Operation..................................27
5.5.1.6-Cation Run (Li+, Na+, NH4+, K+, Mg2+, Ca2+) at Room Temperature Operation Continuation....................28
5.6.Isocratic Elution of Ammonium, Alkali Metals and Alkaline Earth Metals
(Li+, Na+, NH4+, K+, Rb+, Cs+, Mg2+, Ca2+, Sr2+, Ba2+) at 60 °C..................................................................29
5.7.Isocratic Elution of 6-Cations Plus Morpholine..........................................................................................30
5.8.10,000:1 Ratio Sodium to Ammonium at 40 °C ..........................................................................................31
5.9.1:10,000 Ratio Sodium to Ammonium at 40 °C ..........................................................................................33
5.10.Analysis of Tap Water at 40 °C ....................................................................................................................34
5.11.Analysis of Waste Water at 40 °C.................................................................................................................35
5.12.Separation of Methylamines, Group I and Group II Cations and
Ammonium at Room Temperature..............................................................................................................36
5.13.Isocratic vs. Gradient Elution of Common Cations and Amines at 60 °C................................................37
5.14.Gradient Elution of the Six Common Cations plus Mono-, Di-, and Triethanolamines at 60 °C..........39
5.15.Isocratic Elution of the Six Common Cations Plus Manganese at 60 °C..................................................40
5.16.Sample pH at 40 °C........................................................................................................................................41
5.17.Linear Working Range at 40 °C...................................................................................................................42
5.18.Step Change Elution of Ethanolamine and the Common Cations on the IonPac CS16 3-mm...............43
5.19.Diverse Concentration Ratios of Ammonium to Ethanolamine on the
IonPac CS16 3-mm at 40 °C..........................................................................................................................44
5.20.Gradient Elution of Ethanolamine, Hydrazine, and the Common Cations..............................................45
5.21.Gradient Elution of Common Cations and Amines at 60 °C .....................................................................47
5.22.Gradient Elution of Common Cations and Alkanolamines at 60 °C.........................................................48
5.23.Separation of Six Cations on a Capillary CS16 column .............................................................................49
SECTION 6 – TROUBLESHOOTING GUIDE.................................................................................. 50
6.1.High Back Pressure........................................................................................................................................51
6.1.1.Finding the Source of High System Pressure ..................................................................................................51
6.1.2.Replacing Column Bed Support Assemblies...................................................................................................52
6.2.Preparation of Eluents...................................................................................................................................53
6.3.Contamination................................................................................................................................................53
6.3.1.A Contaminated Guard or Analytical/Capillary Column ................................................................................53
6.3.2.Sample Loop and/or Tubing Contamination ...................................................................................................53
6.4.High Background or Noise............................................................................................................................54
6.5.Suppressor Not Suppressing Properly.........................................................................................................55
6.6.Poor Peak Resolution.....................................................................................................................................56
6.6.1.Loss of Peak Efficiency Throughout the Chromatogram................................................................................56
6.6.2.Loss of Resolution Throughout the Chromatogram Due to Shortened Retention Times ................................56
6.6.3.Loss of Early Eluting Peak Resolution............................................................................................................57
6.7.Spurious Peaks...............................................................................................................................................57
6.7.1.Poor Efficiency Using Capillary Columns ......................................................................................................58
APPENDIX A - QUALITY ASSURANCE REPORT......................................................................... 59
APPENDIX B - COLUMN CARE ........................................................................................................ 63
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 4 of 65
SECTION 1 – INTRODUCTION
The IonPac®CS16 5-mm and 3-mm Analytical Columns and the CS16 0.5 x 250 mm (P/N 075401) Capillary Column have
been designed specifically for the analysis of alkali metals, alkaline earth metals, and ammonium at diverse concentration
ratios. The CS16 stationary phase is a high-capacity weak cation exchanger functionalized with carboxylic acid groups
having a high selectivity for hydronium ion. It has both cation exchange and reverse phase properties. The CS16 is solvent-
compatible with 100% aqueous eluents, 100% acetonitrile, or 20% tetrahydrofuran without loss of performance.
CAUTION
!
Do not use alcohols
Formation of esters will occur in the column packing.
This can significantly reduce the column capacity for cation exchange.
Table 1
IonPac CS16/CG16 Packing Specifications
Column Particle
Diameter
µm
Substratea
X-linking
Capacity
%
Column
meq/column Functional Group Hydrophobicity
CS16
5 x 250 mm 5.5 55 8.4 Carboxylic acid Medium
CG16
5 x 50 mm 5.5 55 1.7 Carboxylic acid Medium
CS16
3 x 250 mm 5.5 55 3.0 Carboxylic acid Medium
CG16
3 x 50 mm 5.5 55 0.6 Carboxylic acid Medium
CS16
0.5 x 250 mm 5.5 55 0.084 Carboxylic acid Medium
CG16
0.5 x 50 mm 5.5 55 0.017 Carboxylic acid Medium
a
macroporous (100 Å) divinylbenzene/ethylvinylbenzene polymer
Table 2
CS16/CG16 Operating Parameters
Column Typical Back Pressure
at 1.0 mL/min
Psi (MPa)
Standard
Flow Rate
mL/min
Maximum
Flow Rate
mL/min
CS16 5-mm Analytical < 1,400 (9.65) 1.0 2.0
CG16 5-mm Guard < 450 (3.10) 1.0 3.0
CS16 + CG16 5-mm columns < 1,850 (12.75) 1.0 2.0
CS16 3-mm Analytical < 1,400 (9.65) 0.36 0.72
CG16 3-mm Guard < 450 (3.10) 0.36 1.08
CS16 + CG16 3-mm columns < 1,850 (12.75) 0.36 0.72
CS16 0.5-mm Capillary < 1,400 (9.65) 0.01 0.02
CG16 0.5-mm Capillary
Guard <450 (3.10) 0.01 0.02
CS16 + CG16 0.5-mm
columns <1,850 (12.75) 0.01 0.02
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 5 of 65
Read the system manuals. This manual assumes that you are familiar with the installation and operation of the Dionex Ion
Chromatograph (IC). If you do not understand the operation of the system, take the time to familiarize yourself with the
various system components before beginning an analysis. All instrument manuals are available on the Dionex Literature and
Manuals CD-ROM supplied with this column.
You may need to make a liquid line fitting. The IonPac CS16 Analytical Column and the IonPac CG16 Guard Column
have 10-32 PEEK end fittings for use with ferrule/bolt liquid line fittings. If you have an Ion Chromatograph with Tefzel®
liquid lines having 1/4-28 ThermoFlare fittings, it will be necessary to obtain one or more Tefzel liquid lines with a PEEK
bolt and ferrule fitting on one end and a 1/4-28 ThermoFlare fitting on the other end. See, “Dionex Liquid Line Fittings,” for
detailed instructions on purchasing or making these lines.
Always remember that assistance is available for any problem that may be encountered during the shipment or
operation of Dionex instrumentation and columns through the Dionex North America Technical Call Center at 1-800-
DIONEX-0 (1-800-346-6390) or through any of the Dionex Offices listed in “Dionex Worldwide Offices.”
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 6 of 65
SECTION 2 – THE ION CHROMATOGRAPHY SYSTEM
Condition 3-mm System
Operation Summary 5-mm System Operation Summary 0.5-mm System Operation Summary
Eluent Flow Rate Typically 0.36 mL/min Typically 1.0 mL/min Typically 0.01 mL/min
Cation Self-Regenerating
Suppressor CSRS 300 2-mm (P/N 053949) CSRS 300 4-mm (P/N 053948) CCES 300 (P/N 072053)
Cation Atlas Electrolytic
Suppressor CAES® (P/N 065118)
(max. 25 mM MSA)
CAES®
(P/N 065118)
(max. 25 mM MSA)
N/A
Cation MicroMembrane
Suppressor 300 CMMS 300 2-mm (P/N 056753) CMMS 300 2-mm (P/N 056752) N/A
Regenerant Flow Rate Typically 50-100% of 5-mm
System Typically 10-15 mL/min N/A
Injection Loop 5-25 µL 10-50 µL N/A
System Void Volume Eliminate switching valves,
couplers and the GM-3 Gradient
Mixer. Use only the Microbore
GM-4 (s-mm) Mixer (P/N
049135).
Minimize dead volumes.
Switching valves, couplerscan
be used. Use the GM-2, GM-3,
GM-4 or recommended gradient
mixers.
Use only on an IC System
equipped for capillary analysis.
Pumps Use the
GS50/GP50/GP40/IP20/IP25 in
Microbore Configuration with a
Microbore GM-4
(2-mm) Gradient Mixer.
The GPM-2 can be used for 2-
mm isocratic chromatography at
flow rates of 0.5 mL/min or
greater but cannot be used for 2-
mm gradient chromatography.
NOTE: Use of an EG40 (P/N
053920) or EG50 (P/N 053922)
for gradient applications is
highly recommended for
minimum baseline change when
performing eluent step changes
or gradients.
Use the GP40/GP50/IP20/IP25
in Standard-Bore Configuration.
The GPM-3 Gradient Mixer
should be used for gradient
analysis on systems other than
the GP50 and IP25. The GP40
has an active mixer.
NOTE: Use of an EG40 (P/N
053920) or EG50 (P/N 053922)
for gradient applications is
highly recommended for
minimum baseline change when
performing eluent step changes
or gradients.
Use only on a pump designed
for capillary flow rates, such as
the ICS-5000 Capillary Pump.
Detectors AD25/AD20 Cell (6-mm, 7.5
µL)
P/N 046423
CD25 or ED50/ED40
Conductivity Cell with Shield
(P/N 044132)
CDM-2/CDM-3 Cell
(P/N 042770)
ED40/ED50 Integrated
Amperometry
Either the TS-1 or the TS-2 can
be used with the CDM-2 or the
CDM-3. Do not use the TS-2 or
the TS-1 with the ED50/ED40
or the CD20.
Ensure 30-40 psi back pressure
after the cell.
AD25/AD20 Cell (10-mm, 9
µL)
P/N 049393
CD25 or ED50/ED40
Conductivity Cell with Shield
(P/N 044132)
CDM-2/CDM-3 Cell
(P/N 042770)
ED40/ED50 Integrated
Amperometry
Either the TS-1 or the TS-2 can
be used with the CDM-2 or the
CDM-3. Do not use the TS-2 or
the TS-1 with the ED50/ED40
or the CD20.
Ensure 30-40 psi back pressure
after the cell.
Use only a conductivity detector
designed for capillary flow rates
such as the ICS-5000 Capillary
CD.
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 7 of 65
Table 3
Tubing Back Pressures
Color Dionex
P/N ID inches ID cm Volume mL/ft Back Pressure Psi/ft at 1
mL/min
Back Pressure
Psi/ft at 0.25
mL/min
Back Pressure
Psi/ft at 1
mL/min
Green 044777 0.030 0.076 0.137 0.086 0.021 0.003
Orange 042855 0.020 0.051 0.061 0.435 0.109 0.015
Blue 049714 0.013 0.033 0.026 2.437 0.609 0.081
Black 042690 0.010 0.025 0.015 6.960 1.740 0.232
Red 044221 0.005 0.013 0.004 111.360 27.840 3.712
Yellow 049715 0.003 0.008 0.001 859.259 214.815 28.642
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 8 of 65
SECTION 3 – INSTALLATION
3.1. System Requirements
3.1.1. System Requirements for 0.5 mm Operation
The IonPac CS16 0.5-mm Capillary Guard and Capillary Columns are designed to be run on a Capillary Ion Chromatograph
equipped with Suppressed Conductivity detection. It is recommended to run the Capillary Column only on the ICS-5000
Capillary System for best performance.
3.1.2. System Requirements for 5-mm Operation
The IonPac CS16 5-mm Guard and Analytical Columns are designed to be run on any Dionex Ion Chromatograph equipped
with suppressed conductivity detection. Gradient or isocratic methods should be performed on a gradient pump configured
for microbore operation.
3.1.3. System Requirements for 3-mm Operation
The IonPac CS16 3-mm Guard and Analytical Columns are designed to be run on any Dionex Ion Chromatograph equipped
with suppressed conductivity detection. Gradient or isocratic methods should be performed on a system having a gradient
pump configured for standard bore operation. For alternate detection than conductivity refer to Section 2.
3.1.4. Installation of the Capillary Column
1. Before installing the new separator column, tear off the column label and slide it into the holder on the front of the
cartridge (see Figure 1).
2. For reference, Figure 1 shows the column cartridge after installation of both a capillary guard column and a capillary
separator column. Figure 2 shows the column cartridge after installation of only a capillary separator column.
Separator Column Outlet
Separator Column
Separator Column Inlet
Precision Cut Tubing
Guard Column Outlet
Guard Column
Guard Column Inlet
Precision Cut Tubing
1
2
3
4
5
6
7
8
1
2
34
5
6
7
8
Figure 1
Separator and Guard Columns Installed in Column Cartridge
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 9 of 65
Separator Column Outlet
Separator Column
Separator Column Inlet
Precision Cut Tubing
1
2
3
4
1
2
34
Figure 2
Separator Column Only Installed in Column Cartridge
3. Locate the IC Cube Tubing Kit (P/N 072186) that is shipped with the IC Cube. The tubing kit includes the following
items:
Table 4
Contents of the IC Cube Tubing Kit (P/N 072186)
Part Length /
Quantity Part Number Used To Connect…
Precision cut 0.062-mm
(0.0025-in) ID PEEK tubing,
blue
65 mm
(2.56 in) 072188 50 mm guard column outlet to 250 mm
separator column
inlet
Precision cut 0.062-mm
(0.0025-in) ID PEEK tubing,
blue, labeled
VALVE PORT 3
115 mm
(4.53 in) 072189 Guard column inlet to injection valve
Precision cut 0.062-mm
(0.0025-in) ID PEEK
tubing, blue
75 mm
(2.93 in) 074603 35 mm guard column outlet to 150 mm
separator column
inlet
Precision cut 0.062-mm
(0.0025-in) ID PEEK
tubing, blue, labeled
VALVE PORT 3
210 mm
(8.27 in) 072187 Separator column inlet to injection valve
(if a guard column is
not present)
0.25-mm (0.010-in) ID
PEEK tubing, black 610 mm (24 in) 042690 EG degas cartridge REGEN OUT to
waste (if an EG is not
present)
Fitting bolt, 10-32 hex
double-cone (smaller),
black
3 072949 Connect precision
cut 0.062-mm
(0.0025-in) ID PEEK
tubing
Fitting bolt, 10-32
double-cone (larger),
black
1 043275 Connect 0.25-mm
(0.010-in) ID PEEK
tubing (black)
Ferrule fitting, 10-32
double-cone, tan 4 043276 Use with both sizes of fitting bolts
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 10 of 65
4. Refer to the following figures for the precision cut tubing required for your configuration:
250 mm Separator Column
65 mm (2.56 in)
Precision Cut Tubing
(P/N 072188)
50 mm Guard Column
115 mm (4.53 in)
Precision Cut Tubing
(P/N 072189)
1
2
3
4
1
2
3
4
Figure 3
Tubing Connections for 250-mm Separator Column and 50-mm Guard Column
Separator Column
210 mm (4.5 in)
Precision Cut Tubing
(P/N 072187)
(use with any length
seperator column)
1
2
1
2
Figure 4
Tubing Connections for Separator Column Only
5. Lift up the lid of the column cartridge to open it.
6. Remove the fitting plug from the outlet fitting on the separator column. Orient the fitting with a flat side up (see
Figure 5) and push the fitting into the opening at the front of the column cartridge until it stops.
Figure 5
Column Outlet Fitting Installed in Column Cartridge
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 11 of 65
Document No. 031747-05 © 2010 Dionex Corporation December 2010
NOTE
!
7. Coil the separator column tubing inside the cartridge as shown in Figure 1 or Figure 2. Secure the column tubing and
the inlet fitting in the clips on the column cartridge.
8. Secure the inlet and outlet fittings on the guard column (if used) in the column clips on the lid of the column
cartridge.
9. Route the guard column inlet tubing (if used) or the separator column inlet tubing through the clip on the top edge of
the column cartridge lid.
10. Close the lid (you should hear a click) and route the tubing into the slot on the front of the column cartridge (see
Figure 6).
If the columns are installed correctly, the cartridge lid snaps closed easily. If the lid does not close easily, do not
force it. Open the lid and verify that the columns and tubing are installed correctly and secured in the clips.
Separator Column Outlet
Column Inlet Tubing
1
2
1
2
Figure 6
Column Cartridge Closed

Product Manual for IonPac CS16 Page 12 of 65
3.2. Installing the CR-CTC Trap Column for Use with EGC MSA Cartridge
For IonPac CS16 applications using the MSA cartridge, a CR-CTC Continuously Regenerated Trap Column (P/N 060478 or
072079) should be installed at the EGC eluent outlet to remove trace level cationic contaminants such as ammonium from the
carrier deionized water. See the CR-TC Product Manual (Document No. 031910) for instructions. As an alternative, the
CTC-1 Trap Column (P/N 040192) can be used. The CTC-1 Trap Column will require off-line regeneration. To use the CTC
Cation Trap Column, see Section 3.3.
3.3. Installing the Cation Trap Column for Eluent Step Change or Gradient Operation
For gradient operation, an IonPac Cation Trap Column (CTC-1, P/N 040192, for 5-mm CS16 or CTC (2-mm), P/N 043132
for 3-mm CS16) should be installed between the Gradient Pump and the injection valve. Remove the high pressure Gradient
Mixer if present. The CTC is filled with high capacity cation exchange resin which helps to minimize the baseline shift
caused by increasing cationic contaminant levels in the eluent as the ionic concentration of the eluent is increased over the
course of the gradient analysis. To install the CTC, complete the following steps:
A. Remove the Gradient Mixer. It is installed between the gradient pump pressure transducer and the injection valve.
B. Connect the gradient pump directly to the CTC. Connect a waste line to the CTC outlet and direct the line to a waste
container.
C. Flush the CTC. For the CTC-1 use 200 mL of a 10x eluent concentrate of the strongest eluent required by the
application at a flow rate of 2.0 mL/min. Note that with the guard and analytical columns out of line, there is no
need for flow rate restrictions. For the CTC (2-mm), use 50 mL of a 10x eluent concentrate of the strongest eluent
required by the application at a flow rate of 0.5 mL/min
D. Rinse the CTC with the strongest eluent that will be used during the gradient analysis.
E. Reconnect the CTC. Connect the CTC to the eluent line that is connected to the injection valve inlet.
The background conductivity of your system should be less than 3 µS when 10 mN H2SO4or methanesulfonic acid (MSA) is
being pumped through the chromatographic system with the CSRS in-line and properly functioning. The baseline shift should
be no greater than 1 µS during a gradient concentration ramp from 10 to 40 mM methanesulfonic acid (MSA). If the baseline
shifts are greater than 5 µS after equilibration, the CTC should be cleaned using steps A - E above.
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 13 of 65
3.4. The Injection Loop Table 5
Smallest Injectable Volumes (µL)
Valve Type Using 0.012” ID
Tefzel Tubing Using 0.007” ID Tefzel Tubing Using 0.010” ID PEEK Tubing Using 0.005” ID PEEK Tubing
Dionex
BF2 Valve
(8 µL Internal Volume)
(10 cm Loop)
15.2 10.5 13.1 9.2
Dionex
MicroInject Valve
(10.5 µL Internal Volume)
(14 cm Loop)
20.5 14.0 17.6 12.2
Dionex
Microinjection Valve
Model 9126
(0.8 µL Internal Volume)
(10 cm Loop)
8.0 3.3 5.9 2.0
For most applications on a standard bore analytical system, a 10–50 µL injection loop will be sufficient. Dionex recommends
that a 10 µL injection loop be used to avoid overloading the CS16 5-mm Analytical Column. Generally, do not inject more
than 10 nanomoles (100–200 ppm) of any one analyte onto the 5-mm analytical column. Injecting larger volumes of samples
can result in overloading the column which can affect the detection linearity. This phenomenon will be more prevalent at
higher concentrations of the analytes of interest. In the case of the CS16 3-mm, do not inject more than 4 nanomoles (35–70
ppm) of any one analyte onto the 3-mm analytical column.
3.5. Sample Concentration
The IonPac CG16 Guard Column or the Low-Pressure Trace Cation Concentrator, TCC-LP1, should be used for trace cation
concentration. Trace cation concentrators are used primarily in high purity water analysis. The function of a trace cation
concentrator in these applications is to strip ions from a measured volume of a relatively clean aqueous sample matrix. This
can be accomplished by concentrating large volumes of the sample onto a concentrator column and then using this column in
place of the sample loop. The sample should be pumped into the concentrator column in the OPPOSITE direction of the
eluent flow, otherwise the chromatography will be compromised. This process “concentrates” all cationic analyte species
onto the trace cation concentrator (the TCC-LP1 or the CG16) leading to a lowering of detection limits by 2–5 orders of
magnitude. The unique advantage of the trace cation concentrator (TCC-LP1 or the CG16) for the analytical chemist in these
applications is the capability of performing routine trace analyses of sample matrix ions at ng/L levels without extensive and
laborious sample pretreatment.
The IonPac CG16 5-mm Guard Column (P/N 057574) or the Low-Pressure Trace Cation Concentrator (TCC-LP1, P/N
046027) should be used for sample concentration with the IonPac CS16 5-mm Analytical Column. The IonPac CG16 3-mm
Guard Column (P/N 059595) or the Low-Pressure Trace Cation Concentrator (TCC-LP1, P/N 046027) should be used for
sample concentration with the IonPac CS16 3-mm Analytical Column. For the Trace Cation Concentrator to work with the
CS16 0.5 mm Column use the CG16 0.5 mm Column or the IonSwift MCC-100 (0.5 x 80 mm) or MCC-200 (0.75 x 80 mm)
Concentrator Column.
CAUTION
!
The Trace Cation Concentrator (TCC-2, P/N 043103) should NOT be used for sample concentration. The
TCC-2 column packing is a strong cation exchange resin functionalized with sulfonic acid. The
recommended IonPac CS16 eluents will not properly elute ions concentrated on this column.
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 14 of 65
Document No. 031747-05 © 2010 Dionex Corporation December 2010
NOTE
!
3.6. IonPac CG16 Guard Columns
An IonPac CG16 Guard Column is normally used with the IonPac CS16 Analytical or Capillary Column. Retention times
will increase by approximately 20% when a guard column is placed in-line prior to the analytical/capillary column. A guard
is placed prior to the analytical/capillary column to prevent sample contaminants from eluting onto the analytical/capillary
column. It is easier to clean or replace a guard column than it is an analytical/capillary column. For maximum life of the
analytical/capillary column, the guard column should be changed or replaced as part of a regular maintenance schedule or at
the first sign of performance deterioration. Use the test chromatogram that is shipped with the analytical/capillary column or
the initial application run for a performance benchmark.
3.7. Eluent Storage
IonPac CS16 columns are designed to be used with sulfuric acid or methanesulfonic acid (MSA) eluents. Storage under a
helium atmosphere ensures contamination free operation and proper pump performance (nitrogen can be used if eluents do
not contain solvents).
3.8. Cation Self-Regenerating Suppressor and Cation Capillary Electrolytic Suppressor
Requirements
A Cation Self-Regenerating Suppressor should be used for applications that require suppressed conductivity detection. It is
compatible with solvent containing eluents and aqueous ionic eluents of all concentrations with which the systems and
columns are compatible. Aqueous ionic eluents can be used in all CSRS 300 modes of operation.
Solvent containing eluents must be used in the Chemical Suppression Mode using either the CSRS 300 or
CMMS 300 Suppressor. (If the CSRS 300 is used with solvents, be sure to use TBAOH as regenerant and with
no current applied to the CSRS 300 suppressor)
When the oven is operated at > 40 °C, the suppressor should be placed outside the oven.
If you are installing an IonPac CS16 5-mm Analytical Column, use a CSRS 300 (4-mm, P/N 053948). If you are installing an
IonPac CS16 3-mm Analytical Column, use a CSRS 300 (2-mm, P/N 053949). If you are installing an IonPac CS16 0.5-mm
Capillary Column, use a CCES 300 (P/N 072053).
For detailed information on the operation of the Cation Self-Regenerating Suppressor, see Document No. 031139, the
“Product Manual for the Cation Self-Regenerating Suppressor 300, the CSRS 300 (4-mm) and the CSRS 300 (2-mm).” For
detailed information on the operation of the Cation Capillary Electrolytic Suppressor, see Document No. 065386.
3.9. Cation Atlas Electrolytic Suppressor Requirements
A Cation Atlas Electrolytic Suppressor, CAES®, may be substituted for the CSRS 300 for applications up to 25 µeq/min. For
detailed information on the operation of the Cation Atlas Electrolytic Suppressor, see Document No. 031770, the “Product
Manual for the Cation Atlas Electrolytic Suppressor.”
3.10. Cation MicroMembrane Suppressor Requirements
A Cation Self-Regenerating Suppressor, CSRS 300, should be used for applications that require suppressed conductivity
detection. It is compatible with all solvents in the AutoSuppression External Water Mode (see Section 3.7, “Cation Self-
Regenerating Suppressor Requirements”). A Cation MicroMembrane Suppressor, CMMS, may be substituted for the CSRS
300. For detailed information on the operation of the Cation MicroMembrane Suppressor, see Document No. 034359, the
“Product Manual for the Cation MicroMembrane Suppressor 300, the CMMS 300.”
3.11. Using Displacement Chemical Regeneration (DCR) with the Chemical Suppression Mode
Dionex recommends using the Displacement Chemical Regeneration (DCR) Mode for chemical suppression using
tetrabutylammonium hydroxide (TBAOH) and the Cation MicroMembrane Suppressor (CMMS 300). See the DCR kit
manual, Document P/N 031664, for details.

Product Manual for IonPac CS16 Page 15 of 65
3.12. Using AutoRegen®with the Chemical Suppression Mode
Dionex recommends using an AutoRegen Accessory (P/N 039594) with eluents that do not contain acetonitrile. It
should be used with the CMMS 300. The AutoRegen Accessory saves regenerant preparation time and reduces regenerant
consumption and waste.
Acetonitrile is not compatible with the AutoRegen Cation Regenerant Cartridge. The acetonitrile diffuses
into the TBAOH regenerant, concentrates during recirculation and eventually hydrolyzes to acetate and
ammonia, depleting the capacity of the AutoRegen Cation Regenerant Cartridge. If acetonitrile is used with
suppressed conductivity, a pressurized vessel rather than the AutoRegen must be used.
CAUTION
!
When using an AutoRegen System, the regenerant passes over the hydroxide form anion exchange resin in the AutoRegen
Cation Regenerant Cartridge where specific anionic contaminants (such as chloride ions) are continuously removed from the
regenerant (TBAOH) to restore the salt form of the regenerant to the base form. If solvents are used in the eluent, ionic
contaminants from the solvent component of the eluent which are not removed by the AutoRegen Regenerant Cartridge
slowly accumulate in the regenerant. This results in slowly increasing background conductivity. The rate at which the
background conductivity increases versus the required analysis sensitivity will determine how often the regenerant must be
changed. It is not necessary to change the AutoRegen Regenerant Cartridge until it is completely expended.
Use Dionex Cation Regenerant Solution (TBAOH, 0.1 M tetrabutylammonium hydroxide, P/N 039602). This ensures
maximum system performance. If you are using the AutoRegen Accessory (P/N 039594) equipped with an AutoRegen
Cation Regenerant Cartridge (P/N 039563), prepare 0.5 to 1.0 liter of the regenerant. If you plan to use a pressurized vessel,
prepare several liters.
Equilibrate the AutoRegen Cation Regenerant Cartridge to new regenerant. When replacing the recycled regenerant, the first
200 mL of the regenerant should be pumped to waste before recycling of the regenerant is started. Utilizing AutoRegen in
this manner will allow the use of high regenerant flow rates with the minimum of consumption and waste.
Increase the regenerant flow rate for gradient analysis. To minimize the baseline shift when performing an analysis that
requires a H2SO4or methanesulfonic acid step or linear gradient, a high regenerant flow rate (10–15 mL/min) is required.
3.13. Detector Requirements
See Section 2, “The 5-mm and 3-mm Ion Chromatography System,” system detector, cell and thermal stabilizer
requirements.
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 16 of 65
SECTION 4 – OPERATION
4.1. General Operating Conditions
Column: CS16 0.5-mm Capillary Column (+ CG16 0.5-mm Capillary Guard Column)
CS16 5-mm Analytical Column (+ CG16 5-mm Guard Column);
CS16 3-mm Analytical Column (+ CG16 3-mm Guard Column)
Sample Volume 0.5-mm CS16: 0.4 µL Loop
Sample Volume 5-mm CS16: 25 µL Loop + 0.8 µL Injection valve dead volume
Sample Volume 3-mm CS16: 10 µL Loop + 0.8 µL Injection valve dead volume
Eluent: 30 mM Methanesulfonic acid (MSA)
Eluent Flow Rate CS16 5-mm: 1.0 mL/min
Eluent Flow Rate CS16 3-mm 0.36 mL/min
Eluent Flow Rate CS16 0.5-mm 0.010 mL/min
Temperature: 40 °C
SRS Suppressor: Cation Self-Regenerating Suppressor 300 (4-mm) in AutoSuppression
Recycle Mode for the CS16 5-mm;
for CS16 3-mm use the CSRS 300 (2-mm)
or CES Suppressor: Cation Capillary Electrolytic Suppressor, CCES 300 (0.4-mm)
or MMS Suppressor: Cation MicroMembrane Suppressor, CMMS 300 (2-mm or 4-mm)
MMS Regenerant: Tetrabutylammonium hydroxide (TBAOH)
MMS Mode: Displacement Chemical Regeneration (DCR) Mode is recommended
Expected Background Conductivity: < 3 µS
Storage Solution: Eluent
4.2. Operating Precautions
IonPac CS16 Operation Precautions
Operate below 4,000 psi (27.57 MPa)
Filter and Degas Eluents
Filter Samples
Do not use this column with alcohols
CAUTION
!
4.3. Chemical Purity Requirements
Reliable, consistent and accurate results require eluents free of ionic impurities. Chemicals, solvents and deionized water
used to prepare eluents must be of the highest purity available. Low trace impurities and low particle levels in eluents also
help to protect your ion exchange columns and system components. Dionex cannot guarantee proper column performance
when the quality of the chemicals, solvents and water used to prepare eluents has been compromised.
4.3.1. Deionized Water
The deionized water used to prepare eluents should be Type I Reagent Grade Water with a specific resistance of 18.2
megohm-cm. The deionized water should be free of ionized impurities, organics, microorganisms and particulate matter
larger than 0.2 µm. Filter water with a 0.2 µm filter. Bottled HPLC-Grade Water (with the exception of Burdick & Jackson)
should not be used since most bottled water contains an unacceptable level of ionic impurities.
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 17 of 65
4.3.2. Inorganic Chemicals
Reagent Grade inorganic chemicals should always be used to prepare ionic eluents. Whenever possible, inorganic chemicals
that meet or surpass the latest American Chemical Society standard for purity should be used. These inorganic chemicals will
detail the purity by having an actual lot analysis on each label. The following chemicals will perform reliably:
A. Use Fluka or Aldrich Methanesulfonic Acid (MSA) (>99% pure) or Dionex Methanesulfonic Acid (0.4 M).
B. Use only concentrated sulfuric acid (H2SO4), ACS grade or BAKER INSTRA-ANALYZED®for trace metals.
C. Use Dionex Cation Regenerant Solution, tetrabutylammonium hydroxide (TBAOH), P/N 039602, to ensure
maximum system performance when operating with a CMMS 300, or a CSRS 300 in the Chemical Suppression
Mode. For the DCR Mode, use Dionex TBAOH (P/N 057561).
D. Use deionized water with a specific resistance of at least 18.2 megohm-cm to make all standards, eluents and
regenerants.
4.4. Preparation of Eluent Stock Solution Concentrates
Sulfuric acid (H2SO4) is very corrosive. Methanesulfonic acid (MSA) is also a corrosive and a strong
irritant.
W
ARNING
!
Avoid breathing the vapors.
Always use these reagents in a fume hood. Wear gloves and goggles.
4.4.1. 1.0 N Methanesulfonic Acid (MSA) Stock Solution
A 1.0 N methanesulfonic acid stock solution can be prepared as follows:
A. Weigh out 96.10 g of methanesulfonic acid (MSA, > 99%, P/N 033478).
B. Carefully add this amount to a 1-liter volumetric flask containing about 500 mL of deionized water.
C. Dilute to the mark and mix thoroughly.
4.4.2 0.4 N Methanesulfonic Acid (MSA) Eluent Concentrate
0.4 N Methanesulfonic Acid Eluent Concentrate (P/N 057562 or package of 4, P/N 057568) is available from Dionex
4.4.2. 1.0 N Sulfuric Acid Stock Solution
This solution will be used in the preparation of each of the eluents in Section 5, “Example Applications.”
Calculate the amount (in grams) of concentrated sulfuric acid (H2SO4) that you need to add to a 1 liter volumetric flask by
using the % H2SO4composition stated on the label of the particular bottle of H2SO4you are using. For example, if the H2SO4
concentration is 98%, you need to weigh out 50.04 grams of concentrated H2SO4. Carefully add this amount of H2SO4to a 1-
liter volumetric flask containing about 500 mL of deionized water with a specific resistance of 18.2 megohm-cm. Dilute to
the 1 liter mark and mix thoroughly.
In other words:
FW of H2SO4= 98.08 g
H
2SO4concentration = 98%
Document No. 031747-05 © 2010 Dionex Corporation December 2010

Product Manual for IonPac CS16 Page 18 of 65
Therefore, for a 1 N H2SO4solution, weigh out:
1 liter x 98.08 g x 1 mole x 1 mole x 100 g = 50.04 g
1 mole 2 Eq liter 98 g
4.4.3. Eluent Preparation
________ ________ ________ ________
Eluent: X mN Sulfuric Acid (H2SO4) or Methanesulfonic acid (MSA)
Using the table below, pipet x.0 mL of the 1.0 N H2SO4or 1.0 N MSA eluent concentrate (see Section 5.1, “Preparation of
Eluent Stock Solution Concentrates”) into a 1-L volumetric flask. Dilute to 1-L using deionized water with a specific
resistance of 18.2 megohm-cm. Degas the eluent.
Table 6
mN Eluents from Stock Solutions
mN
H2SO4or MSA # mL
H2SO4or MSA
4 4.0
10 10.0
16 16.0
18 18.0
20 20.0
22 22.0
24 24.0
30 30.0
40 40.0
100 100.0
4.5. Eluents with Solvents
Solvents can be added to the ionic eluents used with IonPac CS16 columns to modify the ion exchange process or improve
sample solubility. The solvents used must be free of ionic impurities. However, since most manufacturers of solvents do not
test for ionic impurities, it is important that the highest grade of solvents available be used. Currently, several manufacturers
are making ultrahigh purity solvents that are compatible for HPLC and spectrophotometric applications. These ultrahigh
purity solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent. Currently at
Dionex, we have obtained consistent results using High Purity Solvents manufactured by Burdick and Jackson and Optima®
Solvents by Fisher Scientific.
When using a solvent in an ionic eluent, column back pressures will depend on the solvent used, concentration of the solvent,
the ionic strength of the eluent and the flow rate used. The column back pressure will vary as the composition of water-
acetonitrile mixture varies. The practical back pressure limit for the IonPac CS16 columns is 4,000 psi (27.57 MPa).
The IonPac CS16 is compatible with the HPLC solvents listed in Table 7, “HPLC Solvents for Use with the CS16 Columns.”
Alcohols, however, should be avoided, since the column capacity for cation exchange may be reduced due to the reversible
formation of esters in the column packing. Solvents and water should be premixed in concentrations which allow proper
mixing by the gradient pump and to minimize outgassing. Ensure that all of the inorganic chemicals are soluble in the highest
solvent concentration to be used during the analysis.
Document No. 031747-05 © 2010 Dionex Corporation December 2010