background image

IonPacAS9-SC

034656-06

Page 24 of 28

6.2.5 Contaminated Hardware

To eliminate the hardware as the source of the high background conductivity, bypass the columns and the suppressor. Pump
deionized water with a specific resistance of 18.2 megohm-cm through the system. The background conductivity should be less
than 2 µS. If it is not, check the detector/conductivity cell calibration by injecting deionized water directly into it. See the
appropriate manual for details.

B. Check to see if the eluent compositions and concentrations are correct. An eluent that is too concentrated will cause

the peaks to elute faster. Prepare fresh eluent. If you are using a gradient pump to proportion the eluent, components
from two or three different eluent reservoirs, the resulting eluent composition may not be accurate enough for the
application. Use one reservoir containing the correct eluent composition to see if this is the problem. This may be a
problem when one of the proportioned eluents is less than 5%.

C. Column contamination can lead to a loss of column capacity because all of the anion exchange sites will no longer be

available for the sample ions. For example, polyvalent anions from the sample or metals may concentrate on the
column. Refer to “Column Care,” for recommended column cleanup procedures.

Possible sources of column contamination are impurities in chemicals and in the deionized water used for eluents or
components of the sample matrix.. Be especially careful to make sure that the recommended chemicals are used. The
deionized water should have a specific resistance of at least 18.2 megohm-cm.

D. Diluting the eluent will improve peak resolution, but will also increase the analytes’ retention times. If a 10% dilution

of the eluent is not 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 and let it equilibrate with eluent for about 30 minutes. The column
is equilibrated when consecutive injections of the standard give reproducible retention times. The original column
capacity should be restored by this treatment, since the contaminants should be eluted from the column. If you need
assistance in solving resolution problems, contact the nearest DIONEX Worldwide Office (see, DIONEX Worldwide
Offices)

6.2.6 A Contaminated Anion Self-Regenerating Suppressor, ASRS-ULTRA

This section describes routine cleanup procedures for the Anion Self-Regenerating Suppressors (ASRS-ULTRA) in the case of
contamination. Consult the Troubleshooting Guide (see Section 4, “Troubleshooting Guide”) to first determine that the system
is operating properly. If the ASRS-ULTRA is determined to be the source of higher than normal back pressure, higher than
anticipated conductivity, decreased suppression capacity or decreased sensitivity, cleaning the membrane may restore the
performance of the system. Use the following procedures to clean the membrane.

Metal Contaminants or Precipitates

NOTE

The suppressor voltage is a good indicator of the resistance across the suppressor. Higher resistance may indicate
contamination of the suppressor. For more information regarding monitoring the voltage, see Document No.
031814-02, “Removal of Iron Contamination from Electrolytic Suppressors.”

A. Turn off the SRS Control unit.

B. Disconnect the analytical (and guard) column(s) from the injection valve and the ASRS-ULTRA. Refer to the specific

analytical column Product 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 ASRS-ULTRA 

REGEN IN

 port.

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...

Отзывы: