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IonPacAS9-SC

034656-06

Page 27 of 28

6.3

Loss of Front End Resolution

If poor resolution or efficiency is observed for the peaks eluting near the system void volume compared to the later eluting peaks,
check the following:

A. Improper eluent concentration may be the problem. Remake the eluent as required for your application. Ensure that

the water and chemicals used are of the required purity.

B. Column overloading may be the problem. Reduce the amount of sample ions being injected onto the analytical column

by either diluting the sample or injecting a smaller volume onto the column.

C. Sluggish operation of the injection valve may be the problem. Check the air pressure and make sure there are no gas

leaks or partially plugged port faces. Refer to the valve manual for instructions.

D. Improperly swept out volumes anywhere in the system prior to the guard and analytical columns may be the problem.

Swap components, one at a time, in the system prior to the analytical column and test for front-end resolution after
every system change.

6.4

Poor Peak Resolution

Poor peak resolution can be due any or all of the following factors.

6.4.1 Loss of Column Efficiency

A. Extra-column effects can result in sample band dispersion, making the peaks' elution less efficient. Make sure you are

using PEEK tubing with an ID of no greater than 0.010" to make all eluent liquid line connections between the injection
valve and the detector cell inlet, and that the tubing lengths are as short as possible. Check for leaks.

B. Check 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 5.1.2, Replacing Column
Bed Support Assemblies). If the resin does not  fill  the column body all the way to the top, it means that  the resin bed
has collapsed, creating a headspace. The column must be replaced.

6.4.2 Poor Resolution Due to Shortened Retention Times

Even with adequate system and column efficiency, resolution of peaks will be compromised if analytes elute too fast.

A. Ensure that the eluent flow rate is equivalent to the flow rate specified by the analytical protocol. Measure the eluent

flow rate after the column using a stopwatch and graduated cylinder.

6.5

Spurious Peaks

A. If the samples contain an appreciable level of polyvalent ions and the column is used with a weak eluent system,

polyvalent anions may contaminate the analytical column. The retention times for the analytes will then decrease and
spurious, inefficient (broad) peaks can show up at unexpected times. Clean the column as indicated in “Column Care.”

B. If you need assistance in determining the best way to clean strongly retained solutes in your specific sample matrix

from the IonPac AS9-SC columns, contact the nearest DIONEX Worldwide Office (see, DIONEX Worldwide
Offices).

C. When an injection valve is actuated, the possibility of creating a baseline disturbance exists. This baseline upset can

show up as a peak of varying size and shape. This will occur when the injection valve needs to be cleaned or retorqued
(see valve manual). Check to see that there are no restrictions in the tubing connected to the valve. Also check the valve

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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