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IonPacAS9-SC

034656-06

Page 18 of 28

5.3

Resolution of Low-Concentration Analytes - EPA Water Matrix

The following example demonstrates the separation of sample analytes having highly variable concentrations. Setting the flow
rate at 1.0 mL/min allows for increased resolution of very low concentration analytes such as bromate, chlorite, and chlorate in
the following EPA water matrix sample.

Sample Loop Volume:

100 µL

Analytical Column:

IonPac AS9-SC Analytical Column

Eluent:

1.8 mM Na

2

CO

3

/1.7 mM NaHCO

3

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, AAES

or MMS Suppressor:

Anion MicroMembrane Suppressor, AMMS III (4-mm)

MMS Regenerant:

25-50 mN H

2

SO

4

Expected Background Conductivity:

12-16 µS

Long-term Storage Solution (> 1 week):

100 mM Sodium Bicarbonate

Short-term Storage Solution (< 1 week):

Eluent

1

2

3

4

5

6

7

8

9

10

2

1

0

-1

µS

0

5

10

15

20

Peaks

mg/L

1.

Fluoride

5.66

2.

Chlorite

0.50

3.

Bromate

0.20

4.

Chloride

45.0

5.

Nitrite

0.06

6.

Bromide

0.08

7.

Chlorate

0.14

8.

Nitrate

42.0

9.

Phosphate

0.17

10. Sulfate

50.0

Figure 3

EPA Water Matrix

Summary of Contents for 043185

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

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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...

Page 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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