Thermo Scientific IonPac CS16 Product Manual
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Thermo Scientific IonPac CS16 Product Manual

Thermo Scientific IonPac CS16 Product Manual

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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
PROD,COL,IP,CS16,5X250MM
PROD,COL,IP,CG16,3X50MM
Old Part Number in this
manual
057573
059595
Updated Part Number to
use for new orders
079805
079931

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Summary of Contents for Thermo Scientific IonPac CS16

  • Page 1 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 Updated Part Number to manual use for new orders PROD,COL,IP,CS16,5X250MM...
  • Page 2 ® IonPac CS16 ® IonPac CG16...
  • Page 3 Product Manual for IonPac CS16 Page 1 of 65 Product Manual ® 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...

  • Page 4: Table Of Contents

    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 ...
  • Page 5 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 ..........................

  • Page 6: Section 1 - Introduction

    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.

  • Page 7: Document No

    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 ®...

  • Page 8: Section 2 - The Ion Chromatography System

    Product Manual for IonPac CS16 Page 6 of 65 SECTION 2 – THE ION CHROMATOGRAPHY SYSTEM Condition 3-mm System 5-mm System 0.5-mm System Operation Summary Operation Summary Operation Summary Eluent Flow Rate Typically 0.36 mL/min Typically 1.0 mL/min Typically 0.01 mL/min...
  • Page 9 Product Manual for IonPac CS16 Page 7 of 65 Table 3 Tubing Back Pressures Color Dionex Volume Back Pressure Back Pressure Back Pressure inches mL/ft Psi/ft at 1 Psi/ft at 0.25 Psi/ft at 1 mL/min mL/min mL/min Green 044777 0.030 0.076...

  • Page 10: Section 3 - Installation

    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.
  • Page 11 Product Manual for IonPac CS16 Page 9 of 65 Separator Column Outlet Separator Column Separator Column Inlet Precision Cut Tubing 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...
  • Page 12 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)
  • Page 13 Product Manual for IonPac CS16 Page 11 of 65 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.

  • Page 14: Installing The Cr-Ctc Trap Column For Use With Egc Msa Cartridge

    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.

  • Page 15: The Injection Loop

    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.

  • Page 16: Ionpac Cg16 Guard Columns

    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).

  • Page 17: Using Autoregen With The Chemical Suppression Mode

    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.

  • Page 18: Section 4 - Operation

    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:...

  • Page 19: Inorganic Chemicals

    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.

  • Page 20: Eluent Preparation

    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.
  • Page 21 Product Manual for IonPac CS16 Page 19 of 65 Table 7 HPLC Solvents for Use with IonPac CS16 Columns Solvent Maximum Operating Concentration Acetonitrile 100% Methanol 2-Propanol Tetrahydrofuran Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 22: Making And Using Eluents That Contain Solvents

    Product Manual for IonPac CS16 Page 20 of 65 4.5.1. Making and Using Eluents that Contain Solvents When mixing solvents with water remember to mix solvent with water on a volume to volume basis. If a procedure requires an eluent of 90% acetonitrile, prepare the eluent by adding 900 mL of acetonitrile to an eluent reservoir. Then add 100 mL of deionized water or eluent concentrate to the acetonitrile in the reservoir.

  • Page 23: Section 5 - Example Applications

    Product Manual for IonPac CS16 Page 21 of 65 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”). Different systems will differ slightly in performance due to slight differences in column sets, system void volumes, liquid sweep-out times of different components and laboratory temperatures.

  • Page 24: Production Test Chromatogram At 40 °C

    Production Test Chromatogram at 40 °C Isocratic elution of cations on the IonPac CS16 Analytical Column has been optimized utilizing a methanesulfonic acid eluent. Using this eluent, the weak carboxylate functionalized packing isocratically separates mono- and divalent cations in a single injection.
  • Page 25 3. Ammonium 0.25 4. Potassium 0.50 µS 5. Magnesium 0.25 6. Calcium 0.50 where 1 mg/L = 1 ppm 0. 1 6 Minutes Figure 8 IonPac CS16 3-mm Production Test Chromatogram Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 26: Reproducing The Production Test Chromatogram Using A Sulfuric Acid Eluent At 40 °C

    When substituting sulfuric acid for methanesulfonic acid, the eluent concentration must be increased to 34 mN sulfuric acid in order to resolve all of the peaks in the production test chromatogram with the runtime within 20 minutes. Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...

  • Page 27: 6-Cations (Li + , Na + , Nh4

    Min u tes Figure 10 IonPac CS16 3-mm 6-Cation Run at 40 °C with an Atlas Suppressor The Cation Atlas Electrolytic Suppressor (P/N 056118) can be used with up to 25 mM Methanesulfonic acid at 1.0 mL/min, as with a CS16 5-mm column.

  • Page 28: 6-Cation Fast Run (Li , Na , Nh , Mg , Ca ) At 40 °C

    µS where 1 mg/L = 1 ppm 0 . 8 0 . 6 0 . 4 0 . 2 Minutes Figure 11 IonPac CS16 5-mm 6-Cation Fast Run at 40 °C Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 29: 6-Cation Run (Li , Na , Nh , Mg , Ca ) At Room Temperature Operation

    2. Sodium 3. Ammonium 4. Magnesium 5. Potassium 6. Calcium where 1 mg/L = 1 ppm Eluent: 36 mM Methanesulfonic acid (MSA) Figure 12 IonPac CS16 5-mm 6-Cation Run at Room Temperature Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 30: 6-Cation Run (Li , Na , Nh , Mg , Ca ) At Room Temperature Operation Continuation

    1 mg/L = 1 ppm 2.96 -0.26 Minutes Eluent: 38 mM Methanesulfonic acid (MSA), 29 °C 9.40 6.18 µS 2.96 -0.26 Minutes Figure 13 IonPac CS16 3-mm 6-Cation Run Optimized for Room Temperature Operation Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 31: Nh , K

    Note that with the higher capacity CS16 column, cesium, a monovalent, elutes after magnesium, a divalent. Column: IonPac CS16 3-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...

  • Page 32: Isocratic Elution Of 6-Cations Plus Morpholine

    , NH , Mg , Morpholine and ) can be completed within 20 minutes. Morpholine is well resolved from magnesium. Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop Eluent: 34 mM Methanesulfonic acid (MSA) Eluent Flow Rate: 1.0 mL/min...

  • Page 33: 10,000:1 Ratio Sodium To Ammonium At 40 °C

    (P/N 040192) be placed between the CELL OUT and the suppressor REGEN IN ports (see chromatogram B). Alternatively, the suppressor can be used in the External Water mode. Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...
  • Page 34 The following shows a ratio of 10,000:1 of sodium to ammonium on the CS16 3-mm using an isocratic eluent. Either a smaller sample loop size than with a CS16 5-mm should be used or the sample should be diluted not to overload the column. Column: IonPac CS16 3-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...

  • Page 35: 1:10,000 Ratio Sodium To Ammonium At 40 °C

    REGEN IN ports when using the CSRS 300 in the AutoSuppression Recycle Mode. Alternatively, the suppressor can be used in the External Water Mode. Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop Trap Column:...

  • Page 36: Analysis Of Tap Water At 40 °C

    48 mN methanesulfonic acid eluent. The approximate calculated 300:1 ratio of sodium-to- ammonium is easy to determine in either case (see peaks 2 and 3). Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...

  • Page 37: Analysis Of Waste Water At 40 °C

    The high capacity CS16 column minimizes the chance to overload the column and offers a greater chance of resolving the sample’s component peaks. Column: IonPac CS16 5-mm Analytical Column (no guard) Sample Volume: 25 µL Loop Sample Dilution: 0.5 : 100...

  • Page 38: Separation Of Methylamines, Group I And Group Ii Cations And Ammonium At Room Temperature

    9. Trimethylamine 1.50 0 . 4 where 1 mg/L = 1 ppm ) 0 . 2 Minutes Figure 21 IonPac CS16 5-mm Methylamine Selectivity with Common Cations Using Two Different Eluents Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 39: Isocratic Vs. Gradient Elution Of Common Cations And Amines At 60 °C

    (such as peak # 10, trimethylamine). The CSRS 300 is placed outside of the column oven. Column: IonPac CS16 3-mm Analytical Column (no guard) Sample Volume: 25 µL Loop...
  • Page 40 Note that the suppressor is placed outside the chromatography oven when temperatures exceed 40 °C as they do here. Column: IonPac CS16 3-mm Analytical Column (no guard) Eluent: 6 mM MSA, gradient from 0 to 13 min to...

  • Page 41: Gradient Elution Of The Six Common Cations Plus Mono-, Di-, And Triethanolamines At 60 °C

    Eluent Generator (EG40) was used to generate the methanesulfonic acid gradient. An elevated temperature of 60 °C is used to improve the resolution of ammonium and ethanolamine. The CSRS 300 is placed outside of the column oven. Column: IonPac CS16 3-mm Analytical Column (no guard) Sample Volume: 25 µL Loop Eluent Source:...

  • Page 42: Isocratic Elution Of The Six Common Cations Plus Manganese At 60 °C

    This separation can be achieved on a CS12A at room temperature using isocratic conditions. The CS16 should be used where disparate concentration ratios of sodium and ammonium besides calcium, magnesium and manganese are to be determined. Column: IonPac CS16 3-mm Analytical Column (no guard) Sample Volume: 25 µL Loop Eluent:...

  • Page 43: Sample Ph At 40 °C

    5.16. Sample pH at 40 °C The IonPac CS16 resin contains relatively weak carboxylic acid cation exchange sites. The ionization of the sites are dependent on the eluent and on the sample pH. Furthermore, because these cation exchange sites are hydronium-selective, the sample pH will have an impact on the elution of the analyte cations from such sites.

  • Page 44: Linear Working Range At 40 °C

    Product Manual for IonPac CS16 Page 42 of 65 5.17. Linear Working Range at 40 °C The higher cation exchange capacity of the CS16 5-mm stationary phase reduces overload with sample concentration. The chromatogram shown in this slide was obtained under standard conditions for this stationary phase (30 mM Methanesulfonic acid, 1 mL/min, 40 °C).

  • Page 45: Step Change Elution Of Ethanolamine And The Common Cations On The Ionpac Cs16 3-Mm

    Product Manual for IonPac CS16 Page 43 of 65 5.18. Step Change Elution of Ethanolamine and the Common Cations on the IonPac CS16 3-mm Ethanolamine is a commonly used corrosion inhibitor in the Power Industry. By using a weaker acidic eluent resolution is improved between ammonium and ethanolamine (peaks #3, 4) so that diverse concentration ratios of these two can be determined using the CS16 column.

  • Page 46: Diverse Concentration Ratios Of Ammonium To Ethanolamine On The Ionpac Cs16 3-Mm At 40 °C

    Product Manual for IonPac CS16 Page 44 of 65 5.19. Diverse Concentration Ratios of Ammonium to Ethanolamine on the IonPac CS16 3-mm at 40 °C Column: IonPac CS16 3-mm Analytical Column Trap Column: IonPac CTC (2-mm) (P/N 043132) located between pump and injection valve Sample Volume: 25 µL Loop...

  • Page 47: Gradient Elution Of Ethanolamine, Hydrazine, And The Common Cations

    Product Manual for IonPac CS16 Page 45 of 65 5.20. Gradient Elution of Ethanolamine, Hydrazine, and the Common Cations Ethanolamine and hydrazine are common additives in Power Plant waters and these together with ammonium, sodium and the other cations need to be carefully monitored. The CS16 3-mm uses lower eluent flow rate than the CS16 5-mm and therefore is better suited for process applications.
  • Page 48 Product Manual for IonPac CS16 Page 46 of 65 1.00 0.90 0.80 Analyte µg/L 1. Lithium 0.70 2. Sodium 500,000 3. Ammonium 0.60 4. Ethanolamine 50 5. Hydrazine 0.50 6. Potassium 0.40 7. Magnesium 8. Calcium 0.30 0.20 Minutes * With this same gradient condition, 20,000:1 concentration ratio of Na...

  • Page 49: Gradient Elution Of Common Cations And Amines At 60 °C

    (last eluting peak). The eluent contained no organic solvent, so the suppressor was used in the eluent recycle mode. The suppressor was placed outside the chromatographic oven as the temperature exceeded 40 °C. Analyte mg/L Column IonPac CS16 3-mm Analytical Column (no guard) 1. Lithium 0.05 Eluent 6 mM MSA, gradient from 0 to 13 min to 2.

  • Page 50: Gradient Elution Of Common Cations And Alkanolamines At 60 °C

    40 °C as they do here. Column: IonPac CS16 3-mm Analytical Column (no guard) Analyte mg/L 1. Lithium 0.05...

  • Page 51: Separation Of Six Cations On A Capillary Cs16 Column

    Product Manual for IonPac CS16 Page 49 of 65 5.23. Separation of Six Cations on a Capillary CS16 column ® CS16 (0.5 mm x 250 mm) Column: IonPac Eluent Source: Capillary EGC-MSA cartridge Eluent: 30 mM MSA Flow Rate: 10 µL/min Peak 1.

  • Page 52: Section 6 - Troubleshooting Guide

    SECTION 6 – TROUBLESHOOTING GUIDE The purpose of the Troubleshooting Guide is to help you solve operating problems that may arise while using IonPac CS16 columns. For more information on problems that originate with the Ion Chromatograph (IC) or suppressor, refer to the Troubleshooting Guide in the appropriate operator’s manual.

  • Page 53: High Back Pressure

    Product Manual for IonPac CS16 Page 51 of 65 6.1. High Back Pressure 6.1.1. Finding the Source of High System Pressure Total system pressure for the IonPac CG16 Guard Column plus the CS16 Analytical Column when using the test chromatogram conditions should be equal or less than 1,850 psi (12.75 MPa). If the system pressure is higher than 1,950 psi (13.44 MPa), it is advisable to determine the cause of the high system pressure.

  • Page 54: Replacing Column Bed Support Assemblies

    Product Manual for IonPac CS16 Page 52 of 65 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. If the bed support is contaminated and/or deformed, it may be the cause of poor efficiency and/or poor peak shape. 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 55: Preparation Of Eluents

    Product Manual for IonPac CS16 Page 53 of 65 6.2. 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.

  • Page 56: High Background Or Noise

    B. Testing for Loop Contamination when Using Carboxylated Cation Exchange Columns A simple test can be performed (when using a column such as the IonPac CS16 which contains a carboxylated resin) with methanesulfonic acid or sulfuric acid to see if the sample loop has been contaminated: 1.

  • Page 57: Suppressor Not Suppressing Properly

    Product Manual for IonPac CS16 Page 55 of 65 A. Make sure that the eluents and regenerant are prepared correctly (see Section 5.2, “Eluent Preparation”). B. Determine if the columns or system are contaminated (see Section 6.3, “A Contaminated Guard or Analytical Column”).

  • Page 58: Poor Peak Resolution

    Product Manual for IonPac CS16 Page 56 of 65 Do not recycle the regenerant through the Cation Regenerant Cartridge if the eluent contains acetonitrile. NOTE G. Non-linear response or loss of sensitivity Indications of carbonate contamination are: 1. A higher ammonium peak than should be expected.

  • Page 59: Loss Of Early Eluting Peak Resolution

    Product Manual for IonPac CS16 Page 57 of 65 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 60: Poor Efficiency Using Capillary Columns

    Product Manual for IonPac CS16 Page 58 of 65 6.7.1. Poor Efficiency Using Capillary Columns Incorrectly installed fittings on capillary tubing can increase void volumes, causing chromatograms with tailing peaks. Figure 33 Tailing Peaks Caused by Incorrectly Installed Capillary Tubing Fittings When connecting a capillary tube fitting, make sure that the ferrule and fitting bolt are at least 2 mm (0.1 in) from the...

  • Page 61: Appendix A - Quality Assurance Report

    Page 59 of 65 APPENDIX A - QUALITY ASSURANCE REPORT Quality Assurance Report - IonPac CS16 Analytical Column - 3 x 250 mm Quality Assurance Report - IonPac CS16 Analytical Column - 5 x 250 mm Quality Assurance Report - IonPac CS16 Capillary Column – 0.5 x 250 mm Document No.
  • Page 62 Product Manual for IonPac CS16 Page 60 of 65 Document No. 031747-05 © 2010 Dionex Corporation December 2010...
  • Page 63 Product Manual for IonPac CS16 Page 61 of 65 Document No. 031747-05 © 2010 Dionex Corporation December 2010...
  • Page 64 Product Manual for IonPac CS16 Page 62 of 65 Document No. 031747-05 © 2010 Dionex Corporation December 2010...

  • Page 65: 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 CS16 Analytical, Capillary or Guard Column is 4,000 psi (27.57 MPa). Do not use alcohols.
  • Page 66 Do not clean the column with alcohols or with basic eluents. CAUTION B. Disconnect the Suppressor from the IonPac CS16 Analytical or Capillary Column. If your system is configured with both a guard column and an analytical column, place the guard behind the analytical column in the eluent flow path.
  • Page 67 E. Equilibrate the column(s) with eluent for at least 30 minutes before resuming normal operation. F. Reconnect the IonPac CS16. Connect the Analytical/Capillary Column outlet to the Suppressor and the inlet to either the IonPac CG16 Guard Column or the Pump Module.

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