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IonPacAS9-SC

034656-06

Page 21 of 28

SECTION 6 - TROUBLESHOOTING GUIDE

The purpose of the Troubleshooting Guide is to help you solve operating problems that may arise while using IonPac AS9-SC
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. If you cannot solve the problem on your own, call the DIONEX
Worldwide Office nearest you (see, DIONEX Worldwide Offices).

6.1

High Backpressure

6.1.1 Finding the Source of High System Pressure

Total system pressure when using the IonPac AG9-SC (4-mm) Guard and AS9-SC (4-mm) Analytical Columns at 1.0 mL/min
should also be less than 1,500 psi when using the test chromatogram conditions. Refer to Section 3.4, Eluent Preparation, to see
how solvent concentration can affect the column operating pressure. If the system pressure is higher than 2,000 psi, it is advisable
to determine the cause of the high system pressure. The system should be operated with a High-Pressure In-Line Filter (P/N
035331) which is positioned between the Gradient Pump pressure transducer and the injection valve. Make sure you have one
in place and that it is not contaminated.

A. Make sure that the pump is set to the correct eluent flow rate. Higher than recommended eluent flow rates will cause

higher pressure. Measure the pump flow rate if necessary with a stop watch and graduated cylinder.

B. Determine which part of the system is causing the high pressure. High pressure could be due to a plugged tubing or

tubing with collapsed walls, an injection valve with a clogged port, a column with particulates clogging the bed
support, a clogged High-Pressure In-Line Filter, the suppressor or the detector cell.

To determine which part of the chromatographic system is causing the problem, disconnect the pump eluent line from
the injection valve and turn the pump on. Watch the pressure; it should not exceed 50 psi. Continue adding system
components (injection valve, column(s), suppressor and detector) one by one, while monitoring the system pressure.
The pressure should increase up to a maximum of 1,500 psi when the column(s) are connected. The Anion
MicroMembrane Suppressor may add up to 100 psi. No other components should add more than 100 psi of pressure.
Refer to the appropriate manual for cleanup or replacement of the problem component.

6.1.2 Replacing Column Bed Support Assemblies

If the column inlet bed support is determined to be the cause of the high backpressure, 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.

A. Disconnect the column from the system.

B. Using two open end wrenches, carefully unscrew the inlet (top) column fitting.

C. Turn the end fitting over and tap it against a benchtop or other hard, flat surface to remove the bed support and seal

assembly. If the bed support must be pried out of the end fitting, use a sharp pointed object such as a pair of tweezers,
but be careful that you 

DO NOT SCRATCH THE WALLS OF THE END FITTING.

 Discard the old bed support

assembly.

D. Place a new bed support assembly into the end fitting. Make sure that the end of the column tube is clean and free of

any particulate matter so that it will properly seal against the bed support assembly. Use the end of the column to
carefully start the bed support assembly into the end fitting.

Содержание 043185

Страница 1: ...for IonPac AG9 SC IonPac AS9 SC...

Страница 2: ...4656 06 Page 1 of 28 PRODUCT MANUAL for the IONPAC AG9 SC GUARD COLUMN 4 x 50 mm P N 043186 IONPAC AS9 SC ANALYTICAL COLUMN 4 x 250 mm P N 043185 DIONEX Corporation 2008 Document No 034656 Revision 06...

Страница 3: ...8 The Anion Atlas Electrolytic Suppressor AAES 8 3 9 The Anion MicroMembrane Suppressor AMMS III 8 3 10 Using AutoRegen with the ASRS ULTRA orthe AMMS III in the Chemical Suppression Mode 8 3 11 Using...

Страница 4: ...21 6 1 1 Finding the Source of High System Pressure 21 6 1 2 Replacing Column Bed Support Assemblies 21 6 2 High Background Or Noise 22 6 2 1 Preparation of Eluents 22 6 2 2 Borate Eluent Precautions...

Страница 5: ...e using standard operating conditions of at least 14 000 plates meter The IonPac AS9 SC can be operated at flow rates up to 3 0 mL min with eluents that have a pH between 2 and 11 Eluents may contain...

Страница 6: ...3 or recommended gradient mixers Pumps Use the GP40 GP50 IP20 IP25 in Standard Bore Configuration The GM 3 Gradient Mixer should be used for gradient analysis on systems other than the GP40 GP50 IP20...

Страница 7: ...DIONEX Worldwide Offices 3 2 The Sample Concentrator The Low Pressure Trace Anion Concentrator Column TAC LP1 P N 046026 the Trace Anion Concentrator Column TAC 2 P N 043101 the Anion MicroConcentrat...

Страница 8: ...ange resin which helps to minimize the baseline shift caused by increasing anionic contaminant levels in the eluent as the ionic concentration of the eluent is increased over the course of the gradien...

Страница 9: ...lytic Suppressor 3 9 The Anion MicroMembrane Suppressor AMMS III An Anion MicroMembrane Suppressor the AMMS III P N 056750 can also be used for applications that require suppressed conductivity detect...

Страница 10: ...e the Anion AutoRegen Regenerant Cartridge until it is completely expended and a sudden jump to very high background conductivity is observed 3 11 Using Displacement Chemical Regernation DCR with the...

Страница 11: ...uppressor 4 2 IonPac AS9 SC Operation Precautions CAUTION Filter and Degas Eluents Filter Samples Eluent pH between 2 and 11 and contains no hydroxide Sample pH between 2 and 13 3 mL min Maximum Flow...

Страница 12: ...ckground conductivity when using sodium carbonate bicarbonate isocratic or borate isocratic and gradient eluents with the AS9 SC columns The following table details the use of the above eluent types T...

Страница 13: ...eparation for Gradient Program 1 Eluent 10 mM H3 BO3 10 mM Na2 B4 O7 Thoroughly dissolve 3 814 g Na2 B4 O7 10 H2 O MW 381 42 g mole plus 0 618 g H3 BO3 MW 61 84 g mole in 700 mL degassed deionized wat...

Страница 14: ...vent concentration to be used during the analysis so that salts do not precipitate outin either the pump or the column Table 6 HPLC Solvents for Use with IonPac AS9 SC Columns Solvent Maximum Operatin...

Страница 15: ...2 5 orders of magnitude The concentrator column is used in lieu of the sample loop Pump the sample onto the concentrator column in the OPPOSITE direction of the eluent flow When using concentration t...

Страница 16: ...ChemicalPurityRequirements After running synthetic standards to calibrate your system you may find that real sample matrices foul your columns For this reason it is always advisable to use a guard col...

Страница 17: ...est Sample Loop Volume 25 L Analytical Column IonPac AS9 SC Analytical Column Eluent 2 0 mM Na2 CO3 0 75 mM NaHCO3 Eluent Flow Rate 2 0 mL min SRS Suppressor Anion Self Regenerating Suppressor ASRS UL...

Страница 18: ...tional resolution can be obtained at lower flow rates see Section 4 4 Resolution of Low Concentration Analytes Sample Loop Volume 25 L Analytical Column IonPac AS9 SC Analytical Column Eluent 1 8 mM N...

Страница 19: ...a2 CO3 1 7 mM NaHCO3 Eluent Flow Rate 1 0 mL min SRS Suppressor Anion Self Regenerating Suppressor ASRS ULTRA 4 mm AutoSuppression Recycle Mode or AES Suppressor Anion Atlas Electrolytic Suppressor AA...

Страница 20: ...22 mM Na2 B4 O7 Eluent Flow Rate 2 0 mL min SRS Suppressor Anion Self Regenerating Suppressor ASRS ULTRA AutoSuppression Recycle Mode or MMS Suppressor Anion MicroMembrane Suppressor AMMS III MMS Reg...

Страница 21: ...ytical Column IonPac AS9 SC Analytical Column Eluent 10 mM H3 BO3 10 mM Na2 B4 O7 with step change at 15 1 minutes to Purge 50 mM H3 BO3 50 mM Na2 B4 O7 Eluent Flow Rate 2 0 mL min SRS Suppressor Anio...

Страница 22: ...with particulates clogging the bed support a clogged High Pressure In Line Filter the suppressor or the detector cell To determine which part of the chromatographic system is causing the problem disco...

Страница 23: ...system is shown below ELUENT EXPECTED BACKGROUND CONDUCTIVITY 1 8 mM Na2 CO3 1 7 mM NaHCO3 14 18 S 5 mM Na2 B4 O7 3 4 S 10 mM Na2 B4 O7 4 6 S 22 mM Na2 B4 O7 5 7 S 6 2 1 Preparation of Eluents A Make...

Страница 24: ...ntisbeingrunthrough the column and then elute as sharp bands when the following strong eluent e g 50 mM borate is pumped through the column Dilute eluent contaminants eluting as sharp bands in the str...

Страница 25: ...sufficient to obtain the desired peak resolution or if the resulting increase in retention times is unacceptable clean the column see Column Care After cleaning the column reinstall it in the system...

Страница 26: ...rate In general the eluent flow rate for 4 mm applications it should be 1 0 mL min Refer to the Anion MicroMembrane Suppressor Product Manual Document No 034449 02 for assistance in determining that t...

Страница 27: ...ct Manual for column cleanup procedures C If you are running in the AutoSuppression External Water Mode turn off the external water and disconnect the external water line from the AAES REGEN IN port I...

Страница 28: ...eck to see if headspace has developed in the guard or analytical column e g due to improper use of the column such as submitting it to high pressures Remove the column s top end fitting see Section 5...

Страница 29: ...ice procedures Small baseline disturbances at the beginning or at the end of the chromatogram can be overlooked as long as they do not interfere with the quantification of the peaks of interest For DX...

Страница 30: ...mum of 10 minutes Cap both ends securely using the plugs supplied with the column COLUMN CLEANUP The following column cleanup protocols have been divided into three general isocratic protocols to remo...

Страница 31: ...guard column can be eluted onto the analytical column and irreversibly damage it If in doubt clean each column separately C Set the pump flow rate to 1 0 mL min D If your eluent contains a solvent th...

Страница 32: ...he outlet line of the AS9 SC Guard Column to a separate waste container CAUTION When cleaning an analytical column and a guard column in series ensure that the guard column is placed after the analyti...

Страница 33: ...uard Column to a separate waste container CAUTION When cleaning an analytical column and a guard column in series ensure that the guard column is placed after the analytical column in the eluent flow...

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