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1、for IonPac AG11 IonPac AS11 IonPac AS11 ManualDocument No. 034791-12Page 1 of 44 PRODUCT MANUAL for the IONPAC AG11 GUARD COLUMN (2 x 50 mm, P/N 044079) (4 x 50 mm, P/N 044078) IONPAC AS11 ANALYTICAL COLUMN (2 x 250 mm, P/N 044077) (4 x 250 mm, P/N 044076) Dionex Corporation 2008 Document No. 034791
2、 Revision 12 7 April 2009 IonPac AS11 ManualDocument No. 034791-12Page 2 of 44 TABLE OF CONTENTS SECTION 1 - INTRODUCTION. 4 SECTION 2 - COMPARISON OF ION CHROMATOGRAPHY SYSTEMS 6 SECTION 3 - INSTALLATION . 8 3.1System Requirements . 8 3.1.1System Requirements for 2-mm Operation 8 3.1.2System Requir
3、ements for 4-mm Operation 8 3.2System Void Volume 8 3.3The AG11 Guard Columns 8 3.4The Sample Concentrator . 8 3.5Installing the CR-ATC Anion Trap Column for Use with EGC II KOH Cartridge 9 3.6The Anion Trap Column, ATC-3 . 9 3.7The Injection Loop. 10 3.7.1The 2-mm System Injection Loop, 215 L . 10
4、3.7.2The 4-mm System Injection Loop, 1050 L10 3.8Eluent Storage . 10 3.9Anion Self-Regenerating Suppressor Requirements 11 3.10Anion MicroMembrane Suppressor Requirements .11 3.11Using Displacement Chemical Regeneration (DCR) with the Chemical Suppression Mode 11 3.12Using AutoRegen .11 3.13Detector
5、 Requirements 11 3.14Using the EG50 or EG40 with AS11 11 SECTION 4 - OPERATION . 12 4.1General Operating Conditions . 12 4.2IonPac AS11 Operation Precautions 12 4.3Chemical Purity Requirements 12 4.3.1Inorganic Chemicals 12 4.3.2Deionized Water 12 4.4Solvents . 13 4.4.1Making Eluents that Contain So
6、lvents . 13 IonPac AS11 ManualDocument No. 034791-12Page 3 of 44 4.5Making Eluents . 14 4.5.1Making Sodium Hydroxide Eluents. 14 4.6Regenerant Preparation for the AMMS III. 15 SECTION 5 - EXAMPLE APPLICATIONS 16 5.1Production Test Chromatogram . 17 5.2Gradient Elution of a Large Number of Inorganic
7、Anions and Organic Acid Anions. 18 5.3Using the EluGen EGC-KOH Cartridge for IonPac AS11 Hydroxide Gradients. 21 5.4How System Void Volume Affects the Length of Time Required for Equilibration to the First Eluent 23 5.5Resolution of Short-Chain Monovalent Organic Acid Anions. 25 5.6Effect of Methano
8、l on IonPac AS11 Selectivity. 26 5.7Gradient Separation of Krebs Cycle Acids. 28 5.8Optimized Separation of Organic Acids in Orange Juice . 30 5.9Effect of Solvent on Inorganic Anions Including Iodide, Thiocyanate, Thiosulfate and Perchlorate . 32 5.10Separation of Polyphosphate Anions 34 5.11Separa
9、tion of High Valency Polycarboxylic Aromatic Acids . 35 5.12Separation of Polygalacturonic Acid Oligomers . 36 SECTION 6 - TROUBLESHOOTING GUIDE. 37 6.1High Back Pressure . 38 6.1.1Finding the Source of High System Pressure 38 6.1.2Replacing Column Bed Support Assemblies .39 6.2High Background or No
10、ise . 39 6.2.1Preparation of Eluents . 40 6.2.2A Contaminated Anion Trap Column, the ATC-3 40 6.2.3A Contaminated Guard or Analytical Column . 40 6.2.4Contaminated Hardware 40 6.2.5A Contaminated Suppressor .40 6.3Poor Peak Resolution . 41 6.3.1Loss of Column Efficiency 41 6.3.2Poor Resolution Due t
11、o Shortened Retention Times 41 6.3.3Loss of Front End Resolution . 42 6.4Spurious Peaks . 42 6.5Small Analyte Peak Areas Observed when Using an ASRS 43 APPENDIX A - COLUMN CARE 44 APPENDIX B - CONFIGURATION . 45 IonPac AS11 ManualDocument No. 034791-12Page 4 of 44 SECTION 1 - INTRODUCTION The lonPac
12、 AS11 2-mm (P/N 044077) and 4-mm (P/N 044076) Analytical Columns are specifically designed to resolve a large number of inorganic anions and organic acid anions from a single sample injection in one gradient run using hydroxide eluent systems. Strongly retained trivalent ions, such as phosphate and
13、citrate, are efficiently eluted in the same run that also gives baseline resolution of the weakly retained monovalent anions fluoride, acetate, formate, and pyruvate. Another benefit of using the AS11 column is the ability to easily change the order of elution of ions with different valences simply
14、by changing the gradient profile. For example, if chromate is present in high enough concentration to interfere with citrate, the citrate peak can be moved ahead of the chromate peak by using a slightly different gradient. The AS11 column provides rapid elution of strongly retained ions such as iodi
15、de, thiocyanate, thiosulfate, and chromate using hydroxide/methanol eluents. The selectivity of the AS11 column makes it possible to rapidly elute strongly retained species such as iodide and thiocyanate in brines without interference from the large chloride peak typical of such samples. Hydroxide i
16、s normally used for gradient elution to minimize background shift. Because of high background conductance, sodium carbonate/bicarbonate eluents are not appropriate for gradient analysis but can be used for isocratic applications. AS11 columns are stable between pH 0 and 14 and are compatible with eluents containing 0-100% organic solvents. Table 1 IonPac AS11/AG11 Packing Specifications ColumnParticleSubstrateaLatexLatexbColumnFunctional GroupHydrophobicity DiameterX-linkingDiameterX-L
