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Dionex IONPAC NG1 Product Manual

Guard column, analytical columns
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PRODUCT MANUAL
IONPAC
®
IONPAC
NS1 ANALYTICAL COLUMN
®
(4 x 250 mm, P/N 035321)
IONPAC
NS1-5µm ANALYTICAL COLUMN
®
(4 x 150 mm, P/N 059568)
QUICKSTART STEPS AND LINKS
Click blue text below to get started.
1.
The standard test eluent for the IonPac NS1 is 3 mM Tetrabutylammonium hydroxide/28%
Acetonitrile. See
Section 3.4, "Preparing Eluents with Solvents".
and working solutions for eluents. See
precautions and chemical purity requirements.
2.
Run the Production Test Chromatogram as a system check. See
Test Chromatogram,"
for details.
3.
See
Section 4, "Applications"
4.
See
"Column Care"
for column cleanup and long-term storage recommendations.
©DIONEX Corporation, 1997-2004
NG1 GUARD COLUMN
(4 x 50 mm, P/N 039567)
Section 3, "Operation,"
for example applications.
Document No. 034024
Revision 06
15 January 2004
Make the required stock
for details. Note operation
Section 4.1.1, "Production

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Summary of Contents for Dionex IONPAC NG1

  • Page 1 Run the Production Test Chromatogram as a system check. See Section 4.1.1, “Production Test Chromatogram,” for details. Section 4, “Applications” for example applications. “Column Care” for column cleanup and long-term storage recommendations. ©DIONEX Corporation, 1997-2004 Document No. 034024 Revision 06 15 January 2004...

  • Page 2: Table Of Contents

    System Requirements .............................. 6 The System Injection Loop, 10 - 15 µL ....................... 6 The IonPac Anion Trap Column ..........................6 The IonPac NG1 Guard Column ........................... 7 Eluent Storage ................................7 Anion Self-Regenerating Suppressor Requirements .................... 7 Detector Requirements ............................8 SECTION 3 - OPERATION ......................
  • Page 3 IonPac NS1 Manual Document No. 034024-06 Page 3 of 35 SECTION 4 - APPLICATIONS ...................... 14 Ion Pair Chromatography ............................ 14 4.1.1 Production Test Chromatogram ..........................15 4.1.2 Separation of Anions by MPIC with Suppressed Conductivity Detection and Solvent ........... 16 4.1.3 Separation of Aliphatic Sulfonic Acids by Ion-Pairing with Suppressed Conductivity (MPIC)......

  • Page 4: Section 1 - Introduction

    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 5 IonPac NS1 Manual Document No. 034024-06 Page 5 of 35 Table 2 NS1/NG1 Operating Parameters Standard Maximum Column Typical Back Pressure Flow Rate Flow Rate psi (MPa) mL/min mL/min NS1 Analytical 900 (6.21) - 1,400 (9.66) NG1 Guard 200 (1.38) - 300 (2.07) NS1 + NG1 columns 1,100 (7.59) - 1,700 (11.73) NS1-5 µm analytical...

  • Page 6: Section 2 - Installation

    The System Injection Loop, 10 - 15 µL For most applications on a 4-mm 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 IonPac NS1 4-mm analytical column. Generally, do not inject more than 10 nanomoles (100–200 ppm) of any one analyte onto the 4-mm analytical column.

  • Page 7: The Ionpac Ng1 Guard Column

    The IonPac NG1 Guard Column An IonPac NG1 Guard Column is normally used with the IonPac NS1 analytical column. Retention times will increase by approximately 20% when a guard column is placed in-line prior to the analytical column. A guard is placed prior to the analytical column to prevent sample contaminants from eluting onto the analytical column.

  • Page 8: Detector Requirements

    IonPac NS1 Manual Document No. 034024-06 Page 8 of 35 Detector Requirements See Section 2, “Ion Chromatography System Operation Summary,” for 4-mm system detector, cell and thermal stabilizer requirements.

  • Page 9: Section 3 - Operation

    Low trace impurities and low particle levels in eluents also help to protect your reversed-phase 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.

  • Page 10: Acid Modifiers

    HPLC and spectrophotometric applications. These ultrahigh purity solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent. At Dionex, we have obtained consistent results using High Purity Solvents manufactured by Burdick and Jackson and Optima® Solvents by Fisher Scientific.

  • Page 11: Eluents For Reversed-Phase And Ion Suppression

    1.0 to 5.0 mM. At higher concentrations, they may be difficult to suppress during conductivity measurements. The following Ion Pair Reagents are available from Dionex: P/N 035360 Tetrabutylammonium hydroxide, 0.1 M TBAOH (MPIC-AR1) P/N 035363 Tetrapropylammonium hydroxide, 0.1 M TPAOH (MPIC-AR2) P/N 035361 Hexanesulfonic acid, 0.1 M HSA (MPIC-CR1)

  • Page 12: Regenerant Preparation For The Amms-Ice Ii

    Suppressor (AMMS-ICE II). Tetramethylammonium hydroxide or potassium hydroxide may be used as alternate regenerants, but cause higher background conductivity and therefore compromise total system performance. For ease of preparation and guaranteed purity, use Dionex Cation Regenerant Solution (P/N 039602). For detailed information on the operation of the AMMS-ICE II, see Document No. 032661.

  • Page 13: Csrs Ultra Ii In Chemical Suppression

    For ease of use and guaranteed high purity, use Dionex Anion Regenerant Concentrate (P/N 037164, 039601) to make regenerant for the ASRS ULTRA II. 3.7.2 CSRS ULTRA II in Chemical Suppression For ease of use and guaranteed high purity, use Dionex Cation Regenerant Concentrate (P/N 039602) to make regenerant for the CSRS ULTRA II. CAUTION Acetonitrile is not compatible with the CSRS ULTRA II in the Chemical Suppression Mode when using an AutoRegen Accessory unit.

  • Page 14: Section 4 - Applications

    IonPac NS1 Manual Document No. 034024-06 Page 14 of 35 SECTION 4 - APPLICATIONS Before attempting any of the following example applications, take the time to ensure that your system is properly configured. Ensure that all of the eluents have been made from high purity reagents and deionized water. All water used in the preparation of eluents should be degassed, deionized water.

  • Page 15: Production Test Chromatogram

    IonPac NS1 Manual Document No. 034024-06 Page 15 of 35 4.1.1 Production Test Chromatogram Isocratic elution of anions on the IonPac NS1 analytical column has been optimized utilizing tetrabutylammonium ion as the ion- pairing agent and acetonitrile as the organic modifier. Using these eluent conditions, highly retained anions can be eluted from the hydrophobic packing of the IonPac NS1.

  • Page 16: Separation Of Anions By Mpic With Suppressed Conductivity Detection And Solvent

    IonPac NS1 Manual Document No. 034024-06 Page 16 of 35 4.1.2 Separation of Anions by MPIC with Suppressed Conductivity Detection and Solvent Ion-pairing can separate monovalent anions, such as chlorate and nitrate, which differ in hydration energy. Because ion pairing has low selectivity for higher valency ions, selected monovalent and higher valency ions can be eluted isocratically on the IonPac NS1 analytical column.

  • Page 17: Separation Of Aliphatic Sulfonic Acids By Ion-Pairing With Suppressed Conductivity (Mpic)

    IonPac NS1 Manual Document No. 034024-06 Page 17 of 35 4.1.3 Separation of Aliphatic Sulfonic Acids by Ion-Pairing with Suppressed Conductivity (MPIC) Ion-pairing can provide excellent selectivity for surface active analytes such as surfactants. The separation of aliphatic sulfonic acids on the IonPac NS1 analytical column can be achieved using tetrabutylammonium ion as the ion-pairing agent with conductivity detection.

  • Page 18: Separation Of Aromatic Sulfonic Acids Using Ion-Pairing With Suppressed Conductivity

    IonPac NS1 Manual Document No. 034024-06 Page 18 of 35 4.1.4 Separation of Aromatic Sulfonic Acids Using Ion-Pairing with Suppressed Conductivity The separation of aromatic sulfonic acids is easily obtained by ion-pairing. The eluent system is identical to that used for the separation of aliphatic sulfonic acids.

  • Page 19: Separation Of Aliphatic Quaternary Ammonium Ions Using Ion-Pairing With Suppressed Conductivity (Mpic)

    IonPac NS1 Manual Document No. 034024-06 Page 19 of 35 4.1.5 Separation of Aliphatic Quaternary Ammonium Ions Using Ion-Pairing with Suppressed Conductivity (MPIC) The separation of a series of aliphatic quaternary ammonium ions can be obtained by using an anionic ion-pair reagent such as nonafluoropentanoic acid.

  • Page 20: Separation Of Alkanolamines Using Ion-Pairing With Suppressed Conductivity (Mpic)

    IonPac NS1 Manual Document No. 034024-06 Page 20 of 35 4.1.6 Separation of Alkanolamines Using Ion-Pairing with Suppressed Conductivity (MPIC) The separation of alkanolamines is also obtained with the use of nonafluoropentanoate ion as the ion-pairing agent. The eluent is suppressed with a CSRS ULTRA II, using 10 mN boric acid as regenerant. The boric acid is added to increase the ionization of the ethanolamines, thereby increasing the conductivity.

  • Page 21: Ion Suppression Chromatography

    IonPac NS1 Manual Document No. 034024-06 Page 21 of 35 Ion Suppression Chromatography This chromatographic technique takes advantage of the effect of pH on the dissociation constants for the for acidic and basic organic species. Depending upon the pKa of an organic ionic molecule, the extent of ionization can be controlled by pH. Because the IonPac NS1 10-µm and NS1-5µm column packings have hydrophobic surfaces, a non-ionic or neutral organic molecule will have a greater affinity for it.

  • Page 22: Water Soluble Vitamins By Ion Pairing / Ion Suppression Chromatography

    IonPac NS1 Manual Document No. 034024-06 Page 22 of 35 4.2.1 Water Soluble Vitamins by Ion Pairing / Ion Suppression Chromatography Column: IonPac NS1-5µm Eluent Conditions: 12 to 48% Acetonitile in 35 minutes 5 mM Octane Sulfonic Acid Flow Rate: 1.0 mL/min Detection: UV 254 nm...

  • Page 23: Separation Of Benzoic Acid And O-Nitrobenzoic Acid

    IonPac NS1 Manual Document No. 034024-06 Page 23 of 35 4.2.3 Separation of Benzoic Acid and o-nitrobenzoic Acid BEFORE AFTER Peaks p-Aminobenzoic acid o-Nitrobenzoic acid Benzoic acid p-Nitrobenzoic acid 2, 3 Figure 9 Separation of Benzoic Acid and o-Nitrobenzoic Acid Using Ion Suppression Chromatography Eluent: 50 mM HCl / 32% Acetonitrile...

  • Page 24: Gradient Separation Of Aliphatic Carboxylic Acids

    IonPac NS1 Manual Document No. 034024-06 Page 24 of 35 4.2.4 Gradient Separation of Aliphatic Carboxylic Acids Ion-suppression chromatography uses an acidic eluent that suppresses ionization of the analytes, allowing separation of weak acids by using a reversed-phase column such as the IonPac NS1. The AMMS-ICE II suppressor regenerant for this ion suppression application is potassium hydroxide.

  • Page 25: Section 5 - Troubleshooting

    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. If you cannot solve the problem on your own, contact the Dionex North America Technical Call Center at 1-800-DIONEX-0 (1-800-346-6390).

  • Page 26: High Back Pressure

    5.1.1 Finding the Source of High System Pressure Total system pressure when using the IonPac NG1 Guard and IonPac NS1 analytical columns at 1.0 mL/min should be less than 1,600 psi (11.03 MPa) when using the eluent used to generate the test chromatogram. Total system pressure when using the IonPac NG1 Guard and IonPac NS1 analytical columns at 2.0 mL/min should also be less than 1,600 psi (11.03 MPa) when using the eluent...

  • Page 27: Replacing Column Bed Support Assemblies

    IonPac NS1 Manual Document No. 034024-06 Page 27 of 35 5.1.2 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 28: Contaminated Anion Trap Column, The Atc-3 (4-Mm)

    5.2.3 Contaminated Guard or Analytical Column Remove the IonPac NG1 Guard and IonPac NS1 analytical columns from the system. If the background conductivity decreases, then one (or both) of these columns is (or are) the cause of the high background conductivity, clean the column as instructed in Appendix B - Column Care.

  • Page 29: Poor Peak Resolution

    IonPac NS1 Manual Document No. 034024-06 Page 29 of 35 2. Test the Anion AutoRegen Regenerant Cartridge to see if it is expended. If the background conductivity is low when freshly prepared regenerant is run through the ASRS or CSRS without an AutoRegen Accessory in-line then the cartridge is expended.

  • Page 30: Loss Of Front End Resolution

    If cleaning and retorquing the valve does not help, replace the valve. Use a Dionex High Pressure Injection Valve (P/ N 037142) or a Dionex High Pressure Inert Valve (P/N 037143) as required.

  • Page 31: Small Analyte Peak Areas

    IonPac NS1 Manual Document No. 034024-06 Page 31 of 35 Small Analyte Peak Areas Assuming that the suppressor is the cause of this problem, small analyte peak areas are a result of running eluent through the suppressor with the power off while using the ASRS ULTRA II in the MPIC Suppression Mode or the CSRS ULTRA II in the AutoSuppression External Water Mode.

  • Page 32: Appendix A - Quality Assurance Report

    IonPac NS1 10µ ® Analytical (4 x 250 mm) Product No. 035321 Serial No. : 6139 Pressure (PSI) : 1250 Date : 8/1/00 7:09:11 AM 6139 Eluent: 28% Acetonitrile 4.00 3.0 mM Tetrabutylammonium hydroxide Flow Rate: 1.0 mL/min 3.00 Detection: Suppressed Conductivity ASRS ®...

  • Page 33: Ionpac Ns1 5Μm

    IonPac NS1 5µ ® Analytical (4 x 150 mm) Product No. 039568 Serial No. : #10 Pressure (PSI) : 1930 Date : 2/21/01 9:13:47 AM Eluent: 26/% Acetonitrile 5.00 4.0 mM Tetrabutylammonium hydroxide Flow Rate: 1.0 mL/min 4.00 Detection: Suppressed Conductivity 3.00 ®...

  • Page 34: Appendix B - Column Care

    IonPac NS1 Manual Document No. 034024-06 Page 34 of 35 APPENDIX B - COLUMN CARE B.1 Recommended Operation Pressures The maximum recommended operating pressure for IonPac NS1 columns is 4,000 psi (27.57 MPa). Operating a column above its recommended pressure limit can cause irreversible loss of column performance. B.2 Column Start-Up The IonPac NS1-5µm is tested with, and shipped in, 26% acetonitrile/4.0 mM tetrabutylammonium hydroxide.

  • Page 35: Choosing The Appropriate Cleanup Solution

    C. Regardless of the cleanup solution chosen, use the following cleanup procedure in Section B.6, “Column Cleanup Procedure,” to clean the IonPac NG1 and IonPac NS1. B.4.2 Column Cleanup Procedure A.

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