Thermo Scientific Dionex IonPac CS14 Guard User manual

Thermo Scientific
Dionex IonPac CS14 Columns
Product Manual
P/N: 034848-10 July 2012
Part of Thermo Fisher Scientific

IonPac CS14 Manual Doc. No. 034848-10 Page 1 of 54
PRODUCT MANUAL
for the
IONPAC CG14 GUARD COLUMN
(2 x 50 mm, P/N 044122)
(4 x 50 mm, P/N 044124)
IONPAC CS14 ANALYTICAL COLUMN
(2 x 250 mm, P/N 044121)
(4 x 250 mm, P/N 044123)
© 2012 Thermo Fisher Scientific
Document No. 034848
Revision 10
July 2012

IonPac CS14 Manual Doc. No. 034848-10 Page 2 of 54
TABLEOFCONTENTS
SECTION 1- INTRODUCTION ....................................................................................................... 5
SECTION2 -COMPARISON OF IONCHROMATOGRAPHYSYSTEMS ............................... 7
SECTION3 -INSTALLATION ......................................................................................................... 9
3.1 SystemRequirements ............................................................................................................................................... 9
3.1.1 SystemRequirements for 2-mm Operation ..................................................................................................................9
3.1.2 SystemRequirements for 4-mm Operation ..................................................................................................................9
3.1.3 SystemVoidVolume ....................................................................................................................................................9
3.2 InstallingtheCationTrapColumnforEluentStepchangeorGradientOperation ............................................... 9
3.3 TheInjectionLoop................................................................................................................................................... 10
3.3.1 The2-mm System Injection Loop, 2 -15 μL .............................................................................................................. 11
3.3.2 The4-mmSystem Injection Loop, 10 - 50μL............................................................................................................. 11
3.4 SampleConcentration ..............................................................................................................................................11
3.5 IonPacCG14GuardColumns .................................................................................................................................11
3.6 EluentStorage ..........................................................................................................................................................11
3.7 CationSelf-RegeneratingSuppressor Requirements............................................................................................11
3.8 CationAtlasElectrolyticSuppressorRequirements............................................................................................. 12
3.9 CationMicroMembraneSuppressorRequirements.............................................................................................. 12
3.10 UsingAutoRegen .................................................................................................................................................... 12
3.11 DetectorRequirements ........................................................................................................................................... 12
SECTION4 -OPERATION ............................................................................................................. 13
4.1 GeneralOperatingConditions ............................................................................................................................... 13
4.2 OperatingPrecautions ........................................................................................................................................... 13
4.3 ChemicalPurityRequirements.............................................................................................................................. 13
4.3.1 DeionizedWater ........................................................................................................................................................ 13
4.3.2 Inorganic Chemicals .................................................................................................................................................. 14
4.3.3 Eluents with Solvents ............................................................................................................................................... 14
4.4 MakingandUsingEluentsthat Contain Solvents ................................................................................................. 15
4.5 SampleConcentration ............................................................................................................................................. 15

IonPac CS14 Manual Doc. No. 034848-10 Page 3 of 54
SECTION5- EXAMPLEAPPLICATIONS.................................................................................... 16
5.1 PreparationofEluentStock SolutionConcentrates .............................................................................................. 16
5.1.1 1.0 M MethanesulfonicAcid (MSA) Stock Solution ................................................................................................ 16
5.1.2 1.0 M TrifluoroaceticAcid (TFA) Stock Solution...................................................................................................... 16
5.1.3 0.1M 18-Crown-6 Ether Stock Solution .................................................................................................................... 16
5.1.4 Pyrophosphoric Acid ................................................................................................................................................ 17
5.2 EluentPreparation .................................................................................................................................................. 17
5.3 ProductionTestChromatogram ............................................................................................................................. 18
5.4 IsocraticElutionofAmmonium,GroupI&IICations ........................................................................................... 19
5.5 TheEffectofSampleAcidityonIonPacCS14Efficiency....................................................................................... 20
5.6 SelectivityControlofMagnesium,Manganeseand Calcium ................................................................................ 21
5.7 Isocratic ElutionofMorpholineandResolutionEnhancementAdditionofSolventtoEluent .............................. 22
5.8 ElutionofMorpholinewithMono-,Di-andTrimethylaminesWithResolutionEnhancementThroughGradient
Elution...................................................................................................................................................................... 24
5.9 IsocraticElutionofMono-,Di-andTrimethylaminesandResolutionEnhancementthroughAdditionofSolventto
Eluent ....................................................................................................................................................................... 25
5.10 ElutionofMono-,Di-andTriethylaminesWithResolutionEnhancementThroughtheAdditionof Solvent to the
Eluent ....................................................................................................................................................................... 26
5.11 GradientElutionofCyclohexylamine ..................................................................................................................... 28
5.12 ElutionofAliphatic Monoamines ............................................................................................................................ 29
5.13 GradientElutionofAlkylamines,Ammonia,GroupI& IICations ....................................................................... 31
5.14 ElutionofDi-andTriethanolamines ....................................................................................................................... 33
5.15 TheIsocraticSeparationofEthanolamineandtheGroupI&IICations .............................................................. 34
5.16 ElutionofSubstitutedMethyl-andEthylaminoethanols ........................................................................................ 35
5.17 MethanesulfonicAcid GradientElutionofAlkanolamineswithAmmonium,GroupI&IICations .................... 36
5.18 Methanesulfonicacid/18-Crown-6Gradient Elution ofAlkanolamineswithGroupI&IICations .................. 38
5.19 TheEffectofTemperatureontheGradientElutionofDiamineswithAmmonia,GroupI&IICations ............... 40

IonPac CS14 Manual Doc. No. 034848-10 Page 4 of 54
SECTION6-TROUBLESHOOTINGGUIDE............................................................................... 42
6.1 High Back Pressure ............................................................................................................................................... 43
6.1.1 Finding the Source of High System Pressure............................................................................................................ 43
6.1.2 Replacing Column Bed SupportAssemblies ............................................................................................................. 44
6.2 Preparation ofEluents ............................................................................................................................................ 45
6.3 AContaminatedGuardorAnalyticalColumn ........................................................................................................ 45
6.4 HighBackgroundor Noise ..................................................................................................................................... 45
6.5 ASuppressorNotSuppressing Properly ............................................................................................................... 46
6.6 PoorPeakResolution ............................................................................................................................................. 47
6.6.1 Loss of Peak Efficiency throughout the Chromatogram............................................................................................ 47
6.6.2 Loss of Resolution Throughout the Chromatogram Due to Shortened Retention Times ......................................... 47
6.6.3 Loss of Early Eluting Peak Resolution ...................................................................................................................... 48
6.7 Spurious Peaks ....................................................................................................................................................... 48
APPENDIXA- QUALITYASSURANCEREPORT....................................................................... 49
APPENDIXB- COLUMNCARE .................................................................................................. 52
RecommendedOperatingPressures ................................................................................................................................ 52
ColumnStart-Up ................................................................................................................................................................ 52
ColumnStorage ................................................................................................................................................................. 52
ColumnConditioning......................................................................................................................................................... 52
ColumnCleanup ................................................................................................................................................................ 52
Column Cleanup Procedure for Polyvalent Cations andAcid-Soluble Contaminants or Transition Metals ........................ 53
Hydrophobic Cations and Organic Contaminants ............................................................................................................... 53

IonPac CS14 Manual Doc. No. 034848-10 Page 5 of 54
SECTION 1 - INTRODUCTION
The IonPac®CS14 4-mm (P/N 044123) and 2-mm (P/N 044121) Analytical Columns are designed specifically for the separation
of alkyl and alkanolamines from the Group I and Group II cations. The CS14 stationary phase consists of a 8.0 μm poly
(ethylvinylbenzene/divinylbenzene) macroporous substrate resin that is functionalized with a relatively weak carboxylic acid.
It has both cation exchange and reverse phase properties. It differs from other Dionex cation exchange columns such as the
IonPac CS3, CS10 and CS11, which have a sulfonic acid functionality making them strong cation exchangers. The CS14 is
similar to the CS12 in that both of these stationary phases have carboxylate functionality making them relatively weak cation
exchangers with a high selectivity for hydronium ion. These weak cation exchangers use low ionic strength eluents to
isocratically elute both monovalent and divalent cations in a relatively short period of time without the use of the divalent
eluent modifiers which are necessary for divalent cation elution with the strong cation exchangers. The hydrophilic
characteristic of the surface permit alkyl and alkanolamines to be eluted with good peak symmetry and efficiency. However,
short-chain alkanolamines, such as monoethanolamines, may exhibit improved separations on the IonPac CS12. The IonPac
CS14 Column is compatible with eluents having pH from 0 to 14 and is solvent-compatible. The column can be used with 0-
100% acetonitrile, 0-100% methanol, 0-100% isopropanol, 0-20% tetrahydrofuran or 0-100% aqueous eluents without loss of
performance.
Table 1
IonPac CS14/CG14 Packing Specifications
Column Particle SubstrateaColumn Functional Hydrophobicity
Diameter X-linking Capacity Group
μm % meq/column
CS14 8.0 55 1.3 Carboxylic Low
4 x 250 mm acid
CG14 8.0 55 0.26 Carboxylic Low
4x50mm acid
CS14 8.0 55 0.325 Carboxylic Low
2 x 250 mm acid
CG14 8.0 55 0.065 Carboxylic Low
2x50mm acid
amacroporous (100 Å) divinylbenzene/ethylvinylbenzene polymer
Table 2
CS14/CG14 Operating Parameters
Standard Maximum
Column Typical Back Pressure Flow Rate Flow Rate
psi (MPa) mL/min mL/min
CS14 4-mm Analytical < 1,200 (8.27) 1.0 3.0
CG14 4-mm Guard < 450 (3.10) 1.0 3.0
CS14 + CG14 4-mm columns < 1,650 (11.37) 1.0 3.0
CS14 2-mm Analytical < 1,200 (8.27) 0.25 1.0
CG14 2-mm Guard < 450 (3.10) 0.25 1.0
CS14 + CG14 2-mm columns < 1,650 (11.37) 0.25 1.0

IonPac CS14 Manual Doc. No. 034848-10 Page 6 of 54
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.”
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.
You may need to make a liquid line fitting. The IonPac CS14 Analytical Column and the IonPac CG14 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.

IonPac CS14 Manual Doc. No. 034848-10 Page 7 of 54
SECTION 2 - COMPARISON OF ION CHROMATOGRAPHY SYSTEMS
The proper configuration of 2-mm system injection volume, mass loading, system void volume and flow rate is based on the
ratio of the 2-mm to 4-mm column cross-sectional area which is a factor of 1/4.
CONFIGURATION 2-mm 4-mm
Eluent Flow Rate 0.25 mL/min 1.0 mL/min
SRS CSRS® ULTRA (2-mm)
(P/N 053949)
CSRS® ULTRA (4-mm)
(P/N 053948)
MMS CMMS III (2-mm)
(P/N 056753)
CMMS III (4-mm)
(P/N 056752)
AES CAES®
(P/N 056118)
CAES®
(P/N 056118)
NOTE
Do not run suppressors over 40°C. If application requires a higher temperature, place
suppressor outside of chromatographic oven.
Regenerant Flow Rate See suppressor manual. See suppressor manual.
Injection Loop 2 - 15 µL
Use the Rheodyne
Microinjection Valve,
Model No. 9126 DIONEX
P/N 044697) for full loop
injections <15 µL.
10 - 50 µL
System Void Volume Eliminate switching valves,
couplers and the GM-3
Gradient Mixer. Use only
the Microbore GM-4 (2-
mm) Mixer (P/N 049135).
Minimize dead volumes.
Switching valves, couplers
can be used. Use the GM-2 ,
GM-3 or recommended
gradient mixers.
Pumps Use the
GS50/GP50/GP40/IP20/IP2
5 in Microbore
Configuration with a
Microbore GM-4 (2-mm)
Gradient Mixer.
No External Gradient Mixer
is required for
GS50/GP50/GP40 Pump
when performing gradient
analysis
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
Use the
GP40/GS50/GP50/IP20/IP2
5 in Standard-Bore
Configuration.
The GM-3 Gradient Mixer
should be used for gradient
analysis on systems other
than the
GP40/GP50/IP20/IP25 and
the DX-300 HPLC Pump.

IonPac CS14 Manual Doc. No. 034848-10 Page 8 of 54
Table3
Tubing Back Pressures
CONFIGURATION 2-mm 4-mm
Detectors AD20/AD25 Cell
(6-mm, 7.5 µL, P/N
046423)
VDM-2 Cell
(3-mm, 2.0 µL, P/N
043120)
CD20, CD25, CD25A,
ED40, ED50, or ED50A
Conductivity Cell with DS3
P/N 044130 or
Conductivity Cell with
shield
P/N 044132
CDM-2/CDM-3 Cell
P/N 042770
Replace the TS-1 with the
TS-2 (P/N 043117) on the
CDM-2 or the CDM-3. The
TS-2 has been optimized for
2-mm operation. Do not use
the TS-2 or the TS-1 with
the ED40/ED50/ED50A or
the CD20/CD25/CD25A.
Ensure 30-40 psi back
pressure after the cell (see
Table 3).
AD20/AD25 Cell
(10-mm, 9 µL, P/N 049393)
VDM-2 Cell (6-mm, 10 µL)
P/N 043113
CD20, CD25, CD25A,
ED40, ED50, or ED50A
Conductivity Cell with DS3
P/N 044130 or with shield
P/N 044132
CDM-2/CDM-3 Cell
P/N 042770
Either the TS-1 with 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
ED40/ED50/ED50A or the
CD20/CD25/CD25A.
Ensure 30-40 psi back
pressure after the cell (see
Table 3).
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/cm 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

IonPac CS14 Manual Doc. No. 034848-10 Page 9 of 54
SECTION 3 - INSTALLATION
3.1 System Requirements
3.1.1 System Requirements for 2-mm Operation
The IonPac CS14 2-mm Guard and Analytical Columns are designed to be run on the following Dionex Ion Chromatographs
equipped with suppressed conductivity detection. Isocratic analyses at flow rates of 0.5 mL/min or greater can be performed
on a pump with standard (1/8" pistons) pump heads. For isocratic analyses at flow rates below 0.5 mL/min and gradient
analyses, a microbore pump (1/16" pistons) must be employed.
3.1.2 System Requirements for 4-mm Operation
The IonPac CS14 4-mm Guard and Analytical Columns are designed to be run on any Dionex Ion Chromatograph equipped
with suppressed conductivity detection. Gradient methods and methods requiring solvent containing eluents should be
performed on a system having a pump with standard 1/8" pump heads. Isocratic analysis can also be performed on a standard
bore pump.
3.1.3 System Void Volume
When using 2-mm columns, it is particularly important to minimize system void volume. The system void volume should be
scaled down to at least 1/4 of the system volume in a standard 4-mm system. For best performance, all of the tubing installed
between the injection valve and detector should be 0.005" (P/N 044221) ID PEEK tubing. 0.010" ID PEEK tubing (P/N 042260)
or 0.012" Tefzel tubing (see “Dionex Product Selection Guide”) may be used but peak efficiency will be compromised which
may also result in decreased peak resolution. Minimize the lengths of all connecting tubing and remove all unnecessary
switching valves and couplers. If you need assistance in properly configuring your system contact the Dionex Office nearest
you (see, “Dionex Worldwide Offices”).
3.2 Installing the Cation Trap Column for Eluent Step change or Gradient Operation
An IonPac Cation Trap Column (CTC (2-mm), P/N 043132 or CTC-1 (4-mm), P/N 040192) 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 (2-mm) or CTC-1 (4-mm), 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. 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 2-mm flow rate
restrictions.
D. Rinse the CTC with the strongest eluent that will be used during the gradient analysis.