Thermo Scientific Dionex IonPac CS14 Guard Product Manual
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Thermo Scientific Dionex IonPac CS14 Guard Product Manual

Thermo Scientific Dionex IonPac CS14 Guard Product Manual

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

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  • Page 1 Thermo Scientific Dionex IonPac CS14 Columns Product Manual P/N: 034848-10 July 2012 Part of Thermo Fisher Scientific...
  • Page 2 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) ©...

  • Page 3: Table Of Contents

    IonPac CS14 Manual Doc. No. 034848-10 Page 2 of 54 TABLE OF CONTENTS SECTION 1 - INTRODUCTION ....................... 5 SECTION 2 - COMPARISON OF ION CHROMATOGRAPHY SYSTEMS ....... 7 SECTION 3 - INSTALLATION ......................9 System Requirements ............................... 9 3.1.1 System Requirements for 2-mm Operation ........................9 3.1.2 System Requirements for 4-mm Operation ........................
  • Page 4 IonPac CS14 Manual Doc. No. 034848-10 Page 3 of 54 SECTION 5 - EXAMPLE APPLICATIONS ..................16 Preparation of Eluent Stock Solution Concentrates ....................16 5.1.1 1.0 M Methanesulfonic Acid (MSA) Stock Solution ....................16 5.1.2 1.0 M Trifluoroacetic Acid (TFA) Stock Solution ...................... 16 5.1.3 0.1 M 18-Crown-6 Ether Stock Solution ........................
  • Page 5 IonPac CS14 Manual Doc. No. 034848-10 Page 4 of 54 SECTION 6 - TROUBLESHOOTING GUIDE ................42 High Back Pressure ............................... 43 6.1.1 Finding the Source of High System Pressure ......................43 6.1.2 Replacing Column Bed Support Assemblies ......................44 Preparation of Eluents ............................

  • Page 6: Section 1 - Introduction

    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.
  • Page 7 IonPac CS14 Manual Doc. No. 034848-10 Page 6 of 54 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.

  • Page 8: Section 2 - Comparison Of Ion Chromatography Systems

    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...
  • Page 9 IonPac CS14 Manual Doc. No. 034848-10 Page 8 of 54 CONFIGURATION 2-mm 4-mm Detectors AD20/AD25 Cell AD20/AD25 Cell (6-mm, 7.5 µL, P/N (10-mm, 9 µL, P/N 049393) 046423) VDM-2 Cell (6-mm, 10 µL) VDM-2 Cell P/N 043113 (3-mm, 2.0 µL, P/N 043120) CD20, CD25, CD25A, CD20, CD25, CD25A,...

  • Page 10: Section 3 - Installation

    IonPac CS14 Manual Doc. No. 034848-10 Page 9 of 54 SECTION 3 - INSTALLATION 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.

  • Page 11: The Injection Loop

    IonPac CS14 Manual Doc. No. 034848-10 Page 10 of 54 Reconnect the CTC. Connect the CTC to the eluent line that is connected to the injection valve. The background conductivity of your system should be less than 3 µS when 10 mM methanesulfonic acid (MSA) is being pumped through the chromatographic system with the CSRS in-line and properly functioning.

  • Page 12: The 2-Mm System Injection Loop, 2 - 15 Μl

    IonPac CS14 Manual Doc. No. 034848-10 Page 11 of 54 3.3.1 The 2-mm System Injection Loop, 2 - 15 μL For most applications on a 2-mm analytical system, a 2–15 µL injection loop is sufficient. Dionex recommends that a 2.5 µL injection loop be used to avoid overloading the CS14 2-mm Analytical Column.

  • Page 13: Cation Atlas Electrolytic Suppressor Requirements

    IonPac CS14 Manual Doc. No. 034848-10 Page 12 of 54 If you are installing an IonPac CS14 2-mm Analytical Column, use a CSRS ULTRA (2-mm, P/N 043188). For detailed information on the operation of the Cation Self-Regenerating Suppressor ULTRA, see Document No. 031370, the “Product Manual for the Cation Self-Regenerating Suppressor ULTRA, the CSRS ULTRA.”...

  • Page 14: Section 4 - Operation

    IonPac CS14 Manual Doc. No. 034848-10 Page 13 of 54 SECTION 4 - OPERATION General Operating Conditions Sample Volume: 2-mm: 2.5 µL Loop + 0.8 µL Injection valve dead volume 4-mm: 25 µL Loop + 0.8 µL Injection valve dead volume Column: 2-mm: CS14 2-mm Analytical Column (+ CG14 2-mm Guard Column) 4-mm: CS14 4-mm Analytical Column (+ CG14 4-mm Guard Column)

  • Page 15: Eluents With Solvents

    IonPac CS14 Manual Doc. No. 034848-10 Page 14 of 54 B. Use Fluka or Aldrich Methanesulfonic Acid (MSA) (>99% pure). C. In the Chemical Suppression Mode of operation, use Dionex Cation Regenerant Solution (tetrabutylammonium hydroxide (TBAOH), P/N 039602) to ensure maximum system performance when operating with a CSRS ULTRA (4- mm) or (2-mm).

  • Page 16: Making And Using Eluents That Contain Solvents

    IonPac CS14 Manual Doc. No. 034848-10 Page 15 of 54 CAUTION When purging or degassing eluents containing solvents, do not purge or degas the eluent excessively since it is possible that a volatile solvent can be “boiled” off from the solution. Always degas and store all eluents in glass or plastic eluent bottles pressurized with helium.

  • Page 17: Section 5 - Example Applications

    IonPac CS14 Manual Doc. No. 034848-10 Page 16 of 54 SECTION 5 - EXAMPLE APPLICATIONS The chromatograms in this section were obtained using columns that reproduced the Production test Chromatogram (see Section 5.3, “Production Test Chromatogram”) on optimized Ion Chromatographs (see Section 3, “Installation”).

  • Page 18: Pyrophosphoric Acid

    IonPac CS14 Manual Doc. No. 034848-10 Page 17 of 54 5.1.4 Pyrophosphoric Acid A 5.45 mM Pyrophosphoric acid solution can be prepared as follows: Add 0.97 g pyrophosphoric acid (MW = 177.98). Dilute to a final volume of 1 L using deionized water. Degas the eluent.

  • Page 19: Production Test Chromatogram

    IonPac CS14 Manual Doc. No. 034848-10 Page 18 of 54 Production Test Chromatogram Isocratic elution of amines and inorganic cations on the IonPac CS14 Analytical Column has been optimized utilizing methanesulfonic acid because of its suitability for use with the Cation Self-Regenerating Suppressor CSRS ULTRA (4-mm and 2-mm).

  • Page 20: Isocratic Elution Of Ammonium, Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 19 of 54 Isocratic Elution of Ammonium, Group I & II Cations Resolution of Group I and Group II Cations (Li , Na , NH , Rb , Cs , Mg , Ca , Sr , Ba ) is accomplished by isocratic...

  • Page 21: The Effect Of Sample Acidity On Ionpac Cs14 Efficiency

    IonPac CS14 Manual Doc. No. 034848-10 Page 20 of 54 The Effect of Sample Acidity on IonPac CS14 Efficiency The IonPac CS14 packing is functionalized with a unique carboxylate functional group that ensures long-term column stability. The column is compatible with acidic eluents and samples. The performance of the CS14 does not deteriorate with the injection of acidic samples up to approximately 20 mM in hydronium ion, thus acid digest or preserved samples can be injected without pH adjustment.

  • Page 22: Selectivity Control Of Magnesium, Manganese And Calcium

    IonPac CS14 Manual Doc. No. 034848-10 Page 21 of 54 Selectivity Control of Magnesium, Manganese and Calcium On-line monitoring of soluble manganese is a good indicator of corrosion in nuclear power plants. Manganese can be quantified in power cooling waters using the IonPac CS14. Pyrophosphoric acid is added to the methanesulfonic acid eluent to enhance the resolution of manganese from magnesium and calcium.

  • Page 23: Isocratic Elution Of Morpholine And Resolution Enhancement Addition Of Solvent To Eluent

    IonPac CS14 Manual Doc. No. 034848-10 Page 22 of 54 Isocratic Elution of Morpholine and Resolution Enhancement Addition of Solvent to Eluent The organic solvent, acetonitrile, can be used to control the IonPac CS14 cation exchange selectivity of morpholine and methyl amines.
  • Page 24 IonPac CS14 Manual Doc. No. 034848-10 Page 23 of 54 Isocratic Eluent: 10 mM MSA / 1.2% ACN Analyte mg/L CSRS ULTRA: AutoSuppression External Water Mode 10.0 Morpholine 50.0 μS 10.0 1 mg/L = 1 ppm Minutes Analyte mg/L Isocratic Eluent: 9 mM MSA CSRS ULTRA: AutoSuppression Recycle Mode...

  • Page 25: Elution Of Morpholine With Mono-, Di- And Trimethylamines With Resolution Enhancement Through Gradient Elution

    IonPac CS14 Manual Doc. No. 034848-10 Page 24 of 54 Elution of Morpholine with Mono-, Di- and Trimethylamines With Resolution Enhancement Through Gradient Elution The determination of morpholine in the presence of mono-, di- and trimethylamines, ammonia, alkali and alkaline earth metals can be accomplished by isocratic elution with 10 mM MSA and 0.3% acetonitrile.

  • Page 26: Isocratic Elution Of Mono-, Di- And Trimethylamines And Resolution Enhancement Through Addition Of Solvent To Eluent

    IonPac CS14 Manual Doc. No. 034848-10 Page 25 of 54 Isocratic Elution of Mono-, Di- and Trimethylamines and Resolution Enhancement through Addition of Solvent to Eluent The determination of mono-, di- and trimethylamines in the presence of ammonia, alkali (excluding potassium) and alkaline earth metals can be accomplished by isocratic elution using 10 mM methanesulfonic acid (MSA).

  • Page 27: Elution Of Mono-, Di- And Triethylamines With Resolution Enhancement Through The Addition Of Solvent To The Eluent

    IonPac CS14 Manual Doc. No. 034848-10 Page 26 of 54 5.10 Elution of Mono-, Di- and Triethylamines With Resolution Enhancement Through the Addition of Solvent to the Eluent The determination of mono-, di- and triethylamines in the presence of ammonia, alkali and alkaline earth metals can be accomplished by isocratic elution using 10 mM methanesulfonic acid (MSA).
  • Page 28 IonPac CS14 Manual Doc. No. 034848-10 Page 27 of 54 Isocratic Eluent: 10 mM MSA CSRS ULTRA: AutoSuppression Recycle Mode μS Analyte mg/L Ethylamine 10.0 Minutes Diethylamine 10.0 Triethylamine 50.0 1 mg/L = 1 ppm Gradient Eluent: As listed above CSRS ULTRA: AutoSuppression External Water mode μ...

  • Page 29: Gradient Elution Of Cyclohexylamine

    IonPac CS14 Manual Doc. No. 034848-10 Page 28 of 54 5.11 Gradient Elution of Cyclohexylamine Power water samples are often treated with cyclohexylamine as a corrosion inhibitor. The determination of cyclohexylamine in the presence of ammonia, Group I & II cations can be accomplished by gradient elution using 9 mM methanesulfonic acid (MSA) with 5% acetonitrile (ACN) as the initial eluent and then stepping to 20 mM methanesulfonic acid (MSA) with 8% acetonitrile.

  • Page 30: Elution Of Aliphatic Monoamines

    IonPac CS14 Manual Doc. No. 034848-10 Page 29 of 54 5.12 Elution of Aliphatic Monoamines The determination of aliphatic monoamines in the presence of ammonia, Group I & II cations can be accomplished by isocratic elution using 40 mM methanesulfonic acid (MSA) if complete resolution of ammonia, Group I & II cations is not required. The determination of all of the components requires a step gradient from 6 mM methanesulfonic acid (MSA) with 2% acetonitrile (ACN) to 8 mM methanesulfonic acid (MSA) with 10% acetonitrile (ACN) at 9 minutes.
  • Page 31 IonPac CS14 Manual Doc. No. 034848-10 Page 30 of 54 Analyte mg/L Isocratic Eluent: 40 mM MSA 3,4,5 CSRS ULTRA: AutoSuppression Recycle Mode μ S n-Propylamine tert-Butylamine 12.5 sec-Butylamine 12.5 10. iso-Butylamine 12.5 11. n-Butylamine 37.5 1 mg/L = 1 ppm Minutes Isocratic Eluent: 20 mM MSA / 1.0% ACN Analyte...

  • Page 32: Gradient Elution Of Alkylamines, Ammonia, Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 31 of 54 5.13 Gradient Elution of Alkylamines, Ammonia, Group I & II Cations The determination of many alkylamines in the presence of ammonia, Group I & II cations can be accomplished by gradient elution in which methanesulfonic acid varies from 5 mM to 20 mM and the acetonitrile varies from 2.5% to 8%.
  • Page 33 IonPac CS14 Manual Doc. No. 034848-10 Page 32 of 54 Analyte mg/L Methylamine Ethylamine Dimethylamine 10.0 Trimethylamine 20.0 Propylamine 10. Morpholine 25.0 11. sec-Butylamine 10.0 12. iso-Butylamine 10.0 13. Mg 14. Ca 15. 2-Methylpiperidine 20.0 16. Di-n-propylamine 20.0 17. 3-Methylpiperidine 20.0 18.

  • Page 34: Elution Of Di- And Triethanolamines

    IonPac CS14 Manual Doc. No. 034848-10 Page 33 of 54 5.14 Elution of Di- and Triethanolamines The determination of diethanolamine in the presence of ammonia, alkali and alkaline earth metals can be accomplished by isocratic elution using 9 mM methanesulfonic acid (MSA). Triethanolamine is widely used in personal care products such as shampoos and industrially in scrubber solutions.

  • Page 35: The Isocratic Separation Of Ethanolamine And The Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 34 of 54 5.15 The Isocratic Separation of Ethanolamine and the Group I & II Cations The IonPac CS14 can be used to monitor the amine content in the quality control of chemical additives, process solutions, plating baths, and scrubber solutions.

  • Page 36: Elution Of Substituted Methyl- And Ethylaminoethanols

    IonPac CS14 Manual Doc. No. 034848-10 Page 35 of 54 5.16 Elution of Substituted Methyl- and Ethylaminoethanols Two fairly hydrophilic amino alcohols, methylaminoethanol and ethylaminoethanol, can be determined in the presence of ammonia, Group I & II cations by isocratic elution using 10 mM trifluoroacetic acid (TFA) with 1.0 to 1.5 % acetonitrile. Trifluoroacetic acid is used in this separation instead of methanesulfonic acid as the source of hydronium ions.

  • Page 37: Methanesulfonic Acid Gradient Elution Of Alkanolamines With Ammonium, Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 36 of 54 5.17 Methanesulfonic Acid Gradient Elution of Alkanolamines with Ammonium, Group I & II Cations The determination of alkanolamines is of great interest since these compounds are widely used in chemical and pharmaceutical industries.
  • Page 38 IonPac CS14 Manual Doc. No. 034848-10 Page 37 of 54 Analyte mg/L Ethanolamine Diethanolamine 30.0 Methylaminoethanol Dimethylaminoethanol 10.0 μ S N-Ethyldiethanolamine 30.0 10. Di-iso-Propanolamine 20.0 11. Diethylaminoethanol 20.0 12. Mg 13. Ca 1 mg/L = 1 ppm Minutes Figure 16 Methanesulfonic Acid Gradient Elution of Alkanolamines with Ammonium, Group I &...

  • Page 39: Methanesulfonic Acid / 18-Crown-6 Gradient Elution Of Alkanolamines With Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 38 of 54 5.18 Methanesulfonic acid / 18-Crown-6 Gradient Elution of Alkanolamines with Group I & II Cations The IonPac CS14 can be used to monitor the amine content in the quality control of chemical additives, process solutions, plating baths, and scrubber solutions.
  • Page 40 IonPac CS14 Manual Doc. No. 034848-10 Page 39 of 54 Analyte mg/L Diethanolamine Methylaminoethanol Triethanolamine 200.0 1-(Dimethylamino)-2-propanol 10.0 Diethylaminoethanol 10.0 N-(n-propyl)diethanolamine 30.0 10. Ca 11. Ethanolamine 12. NH μ S 13. K 1 mg/L = 1 ppm * Identified as a sample impurity Minutes Figure 17 Methanesulfonic Acid / 18-Crown-6 Gradient Elution of...

  • Page 41: The Effect Of Temperature On The Gradient Elution Of Diamines With Ammonia, Group I & Ii Cations

    IonPac CS14 Manual Doc. No. 034848-10 Page 40 of 54 5.19 The Effect of Temperature on the Gradient Elution of Diamines with Ammonia, Group I & II Cations The determination of many diamines in the presence of ammonia, Group I & II cations can be accomplished by gradient elution in which methanesulfonic acid varies from 10 mM to 20 mM and the acetonitrile varies from 5% to 15%.
  • Page 42 IonPac CS14 Manual Doc. No. 034848-10 Page 41 of 54 Temperature: 23 °C (Room Temperature) Analyte mg/L µS Cadaverine 50.0 Putrescine 50.0 1,2-Propanediamine 50.0 10. Ethylenediamine 50.0 11. N,N-Diethylethylenediamine 100.0 1 mg/L = 1 ppm Minutes Temperature: 60 °C µS Minutes Figure 18 The Effect of Temperature on the Gradient Elution of...

  • Page 43: Section 6 - Troubleshooting Guide

    IonPac CS14 Manual Doc. No. 034848-10 Page 42 of 54 SECTION 6 - TROUBLESHOOTING GUIDE The purpose of the Troubleshooting Guide is to help you solve operating problems that may arise while using IonPac CS14 columns. For more information on problems that originate with the Ion Chromatograph (IC) or the suppressor, refer to the Troubleshooting Guide in the appropriate operator’s manual.

  • Page 44: High Back Pressure

    IonPac CS14 Manual Doc. No. 034848-10 Page 43 of 54 High Back Pressure 6.1.1 Finding the Source of High System Pressure Total system pressure for the IonPac CG14 (4-mm) Guard Column plus the CS14 (4-mm) Analytical Column when using the test chromatogram conditions should be equal or less than 1,650 psi (11.37 MPa).

  • Page 45: Replacing Column Bed Support Assemblies

    IonPac CS14 Manual Doc. No. 034848-10 Page 44 of 54 6.1.2 Replacing Column Bed Support Assemblies If the column inlet bed support is determined to be the cause of the high back pressure, it should be replaced. To change the inlet bed support assembly, refer to the following instructions, using one of the two spare inlet bed support assemblies included in the Ship Kit.

  • Page 46: Preparation Of Eluents

    IonPac CS14 Manual Doc. No. 034848-10 Page 45 of 54 Preparation of Eluents A. Make sure that the eluents and regenerant are made correctly. B. Make sure that the eluents are made from chemicals with the recommended purity. C. Make sure that the deionized water used to prepare the reagents has a specific resistance of 18.2 megohm-cm. A Contaminated Guard or Analytical Column Determine if the column is contaminated.

  • Page 47: A Suppressor Not Suppressing Properly

    IonPac CS14 Manual Doc. No. 034848-10 Page 46 of 54 Typical background conductivity levels, in a properly working system, are shown below: ELUENT EXPECTED BACKGROUND CONDUCTIVITY 20 mN Methanesulfonic acid < 1 µS 50 mN Methanesulfonic acid < 2 µS A Suppressor Not Suppressing Properly If the Cation Self-Regenerating Suppressor or the Cation MicroMembrane Suppressor is causing the problem, refer to Cation Self-Regenerating Suppressor ULTRA Product Manual (Document No.031370), to the Cation Atlas Electrolytic Suppressor...

  • Page 48: Poor Peak Resolution

    IonPac CS14 Manual Doc. No. 034848-10 Page 47 of 54 Dips on either side of an analyte peak's base. Non-linear response or loss of sensitivity may occur when the suppressor is contaminated with carbonate. This contamination is possibly from dissolved carbon dioxide in the DI water. Degassing will help minimize the presence of carbon dioxide in acidic eluents or in DI water.

  • Page 49: Loss Of Early Eluting Peak Resolution

    IonPac CS14 Manual Doc. No. 034848-10 Page 48 of 54 C. Column contamination can lead to a loss of column capacity. This is because all of the cation exchange sites will no longer be available for the sample ions. For example, polyvalent cations from the sample or metals may concentrate on the column.

  • Page 50: Appendix A - Quality Assurance Report

    IonPac CS14 Manual Doc. No. 034848-10 Page 49 of 54 APPENDIX A - QUALITY ASSURANCE REPORT Quality Assurance Report - IonPac CS14 Analytical Column - 2 x 250 mm Quality Assurance Report - IonPac CS14 Analytical Column - 4 x 250 mm...
  • Page 51 IonPac CS14 Manual Doc. No. 034848-10 Page 50 of 54 ® IonPac CS14 Analytical (2 x 250 mm) Product No. 44121 Serial No. : 1774 Pressure (PSI) : 940 Date : 5/13/02 4:08:31 PM 1774 Eluent: 10.0 mM methanesulfonic acid 4.00 Eluent Flow Rate: 0.25 mL/min 3.50...
  • Page 52 IonPac CS14 Manual Doc. No. 034848-10 Page 51 of 54 ® IonPac CS14 Analytical (4 x 250 mm) Product No. 44123 Serial No. : 3118 Pressure (PSI) : 1100 Date : 3/3/00 9:47:05 AM 3118 Eluent: 10.0 mM methanesulfonic acid 6.00 Suppressed Conductivity Detection:...

  • Page 53: Appendix B - Column Care

    IonPac CS14 Manual Doc. No. 034848-10 Page 52 of 54 APPENDIX B - COLUMN CARE Recommended Operating Pressures Operating a column above its recommended pressure limit can cause irreversible loss of column performance. The maximum recommended operating pressure for the IonPac CS14 Analytical or Guard Column is 4,000 psi (27.57 MPa). Formation of esters will occur in the column packing.

  • Page 54: Column Cleanup Procedure For Polyvalent Cations And Acid-Soluble Contaminants Or Transition Metals

    IonPac CS14 Manual Doc. No. 034848-10 Page 53 of 54 Column Cleanup Procedure for Polyvalent Cations and Acid-Soluble Contaminants or Transition Metals A. Prepare 500 mL of 1 M HCl for the cleanup solution. Alternatively prepare 500 mM oxalic acid to remove transition metals such as iron or aluminum contamination.
  • Page 55 IonPac CS14 Manual Doc. No. 034848-10 Page 54 of 54 C. Use the following gradient program to remove hydrophobic cations and organic contaminants. Eluent 1: 100 mM HCl Eluent 2: 90% Acetonitrile in deionized water Time (min) % E1 % E2 20.0 25.0 45.0...

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