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IonPac NS1 Manual

Document No. 034024-06

Page 7 of 35

On the next day, prior to the use of the chromatographic system, rinse the IonPac Trap Column. This will help with equilibration
times.

A. Rinse the TC-1 with 30 mL of the strongest eluent used in the gradient analysis.

B. Reconnect the IonPac Trap Column, after flushing it with eluent, to the eluent line that is connected to the injection

valve.

2.4

The IonPac NG1 Guard Column

An IonPac NG1 Guard Column is normally used with the IonPac NS1 analytical column. Retention times will increase by
approximately 20% when a guard column is placed in-line prior to the analytical column. A guard is placed prior to the analytical
column to prevent sample contaminants from eluting onto the analytical column. It is easier to clean or replace a guard column than
it is an analytical column. Replacing the NG1 Guard Column at the first sign of peak efficiency loss or decreased retention time
will prolong the life of the NS1 analytical column.

2.5

Eluent Storage

IonPac NS1 columns are designed to be used with Tetrabutylammonium hydroxide eluent systems. Storage under a helium
atmosphere ensures contamination free operation and proper pump performance (nitrogen can be used if eluents do not contain
solvents).

2.6

Anion Self-Regenerating Suppressor Requirements

The Anion Self-Regenerating Suppressor (ASRS ULTRA II) is used for eluent suppression of MPIC (ion-pairing) eluents by using
the MPIC Suppression Mode of operation. This suppression mode is a combination of the AutoSuppression External Water Mode
augmented with a chemical regenerant such as sulfuric acid (H

2

SO

4

). The MPIC Suppression Mode uses an applied current and

a constant source of dilute sulfuric acid solution delivered from an AutoRegen Accessory or a pressurized bottle system. The MPIC
Suppression Mode reliably provides suppression of typical eluents for MPIC applications using suppressed conductivity detection.
The ion pair reagents, such as tetrabutylammonium hydroxide (TBAOH), are used in concentrations ranging typically from 1.0
to 5.0 mM. For detailed information on the operation of the ASRS ULTRA II, see Document No. 031956.

The Cation Self-Regenerating Suppressor (CSRS ULTRA II) can be used for suppression of MPIC (ion-pairing) eluents by using
the AutoSuppression External Water Mode of operation or the MPIC Suppression Mode depending on the specific MPIC
application. The MPIC Suppression Mode is a combination of the AutoSuppression External Water Mode augmented with a
chemical regenerant if necessary such as boric acid (H

3

BO

3

). When the CSRS ULTRA II is operating in this mode, it uses an applied

current and a constant source of dilute boric acid solution delivered from a pressurized bottle system. For detailed information on
the operation of the CSRS ULTRA II, see Document No. 031956.

An Anion or Cation Self-Regenerating Suppressor should be used for ion pairing applications that require suppressed conductivity
detection. The ASRS ULTRA II in the MPIC Suppression Mode of operation and the CSRS ULTRA II in the AutoSuppression
External Water or MPIC Suppression Mode of operation are compatible with aqueous ionic eluents of all concentrations with which
the column and system are compatible and with solvent containing eluents up to 40% by volume. For applications requiring solvent
above 40% by volume, the Chemical Suppression Mode of operation must be used. Aqueous ionic eluents can be used in all modes
of operation.

NOTE

When using eluents containing solvent above 40% by volume, the ASRS ULTRA II or CSRS ULTRA II should
be used in the Chemical Suppression Mode.

If you are installing an IonPac NS1 4-mm analytical column for ion pairing chromatography with suppressed conductivity
detection, use an ASRS ULTRA II, 4-mm, (P/N 061561) for Anion-MPIC

 

or the CSRS ULTRA II, 4-mm, (P/N 061563) for Cation-

MPIC.

The AMMS-ICE II (P/N 037107) is used with Ion Exclusion and Ion Suppression Modes of Ion Chromatography. For detailed
information on the operation of the AMMS-ICE II, see Document No. 032661.

Summary of Contents for IONPAC NG1

Page 1: ...eluent for the IonPac NS1 is 3 mM Tetrabutylammonium hydroxide 28 Acetonitrile See Section 3 4 Preparing Eluents with Solvents Make the required stock and working solutions for eluents See Section 3 O...

Page 2: ...irements 9 3 3 1 Inorganic Chemicals 9 3 3 2 Deionized Water 9 3 3 3 Solvents 9 3 3 4 Acid Modifiers 10 3 3 5 Base Modifiers 10 3 4 Preparing Eluents that Contain Solvents 10 3 4 1 Eluents for Reverse...

Page 3: ...2 3 Separation of Benzoic Acid and o nitrobenzoic Acid 23 4 2 4 Gradient Separation of Aliphatic Carboxylic Acids 24 SECTION 5 TROUBLESHOOTING 25 5 1 High Back Pressure 26 5 1 1 Finding the Source of...

Page 4: ...eluent suppressor designed for use with ion exclusion and ion suppression separation modes of ion chromatography Many analytes of interest are neither ionizable nor UV detectable Organic and inorgani...

Page 5: ...Back Pressure Flow Rate Flow Rate psi MPa mL min mL min NS1 Analytical 900 6 21 1 400 9 66 1 0 3 0 NG1 Guard 200 1 38 300 2 07 1 0 3 0 NS1 NG1 columns 1 100 7 59 1 700 11 73 1 0 3 0 NS1 5 m analytica...

Page 6: ...192 The IonPac Trap Column should be installed in place of the high pressure gradient mixer between the gradient pump and the injection valve The IonPac Trap Column is filled with high capacity ion ex...

Page 7: ...usingsuppressedconductivitydetection The ion pair reagents such as tetrabutylammonium hydroxide TBAOH are used in concentrations ranging typically from 1 0 to 5 0 mM For detailed information on the op...

Page 8: ...onPac NS1 Manual Document No 034024 06 Page 8 of 35 2 7 Detector Requirements See Section 2 Ion Chromatography System Operation Summary for 4 mm system detector cell and thermal stabilizer requirement...

Page 9: ...er possible inorganic chemicals that meet or surpass the latest American Chemical Society standard for purity should be used These inorganic chemicals will detail the purity by having an actual lot an...

Page 10: ...rength of the eluent and the flow rate used The column back pressure will vary as the composition of water methanol and water acetonitrile mixture varies The practical back pressure limit for the IonP...

Page 11: ...nts Eluent A 10 solvent 90 water Eluent B 90 solvent 10 water Then by programming the gradient pump properly you can go from 100 Eluent A to 100 Eluent B in a prescribed time This will avoid outgassin...

Page 12: ...ity to increase which can result in a noisy background Most solvents have no affect on the cartridge lifetime In all cases the ionic strength of the eluent determines the lifetime of the AutoRegen Reg...

Page 13: ...ranteed high purity use Dionex Cation Regenerant Concentrate P N 039602 to make regenerant for the CSRS ULTRA II CAUTION Acetonitrile is not compatible with the CSRS ULTRA II in the Chemical Suppressi...

Page 14: ...ese ion pair reagents can be anionic or cationic Here is a partial list of typical ion pair reagents A Cationic Tetramethyl ethyl propyl and butyl ammonium salts of the general form R R N R R Counter...

Page 15: ...ng of the IonPac NS1 To guarantee that all IonPac NS1 analytical columns meet high quality and reproducible performance specification standards all columns undergo the following production control tes...

Page 16: ...Detection and Solvent Ion pairing can separate monovalent anions such as chlorate and nitrate which differ in hydration energy Because ion pairing has low selectivity for higher valency ions selected...

Page 17: ...furic acid regenerant Aliphatic sulfonic acids are UV transparent but well detected by suppressed conductivity Column IonPac NS1 10 m Eluent 2 mM Tetrabutylammoniumhydroxide 24 to 48 Acetonitrile in 1...

Page 18: ...atic sulfonic acids Column IonPac NS1 10 m Eluent 2 mM Tetrabutylammonium hydroxide 24 to 48 Acetonitrile in 10 min Flow Rate 1 0 mL min Injection Loop 50 L Detection Suppressed conductivity ASRS ULTR...

Page 19: ...nitrile increases a decrease in the background conductivity is observed Column IonPac NS1 10 m Eluent 2 mM Nonafluoropentanoic acid 20 to 80 Acetonitrile in 10 min Flow Rate 1 0 mL min Injection Loop...

Page 20: ...rate counter ion displaces the hydroxide counter ion from the fully ionized alkali and alkaline earth metals which reduces the observed conductance for these ions Column IonPac NS1 10 m Eluent 2 mM No...

Page 21: ...4 Basic molecules can be deprotonated at high pH s 9 O OH H Anionic R C O R C O pH 4 OH Cationic R NH3 R NH2 H2 0 pH 9 Ionic Neutral Additionally selectivity can be effected by working within one pH u...

Page 22: ...uble Vitamins by Ion Suppression Ion Pair Chromatography Peaks 1 Ascorbic acid 2 Nicotinic acid 3 Nicotinamide 4 Riboflavin 5 Pyridoxine 6 PABA 7 Folic acid 8 Pyridoxamine 9 Thiamine 10 Cyanocobalamin...

Page 23: ...acid 4 2 3 Separation of Benzoic Acid and o nitrobenzoic Acid Figure 9 Separation of Benzoic Acid and o Nitrobenzoic Acid Using Ion Suppression Chromatography BEFORE AFTER Eluent 3 mM HCl 32 Acetonit...

Page 24: ...ydroxide Column IonPac NS1 Flow Rate 1 0 mL min Eluent 1 24 ACN 6 MeOH 0 03 mM HCl Eluent 2 60 ACN 24 MeOH 0 05 mM HCl Gradient 0 100 E2 in 20 min Temperature 42 C Detection Suppressed Conductivity AM...

Page 25: ...dules Disconnect Replace System Module Manual High Background Conductivity Bad Eluents Remake Eluents 5 2 5 2 1 Contaminated Columns Clean Column 5 2 2 5 2 3 Contaminated ASRS or AMMS Clean Suppressor...

Page 26: ...nstall two adaptor assemblies on the filter On the end of the filter with the 1 4 28 male fitting place a 1 4 28 to 10 32 union P N 042806 On the end of the filter with the 1 4 28 female port place a...

Page 27: ...into the end fitting IonPac NS1 Column 4 mm Part P N Analytical Column 10 m 035321 Analytical Column 5 m 039568 Guard Column 039567 Bed Support Assembly 042955 End Fitting 052809 CAUTION If the column...

Page 28: ...minatethehardwareasthesourceofthehighbackgroundconductivity bypasstheSRSsuppressorandpumpdeionizedwater with a specific resistance of 18 2 megohm cm through the system The background conductivity shou...

Page 29: ...lumn must be replaced 5 3 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 Checkt...

Page 30: ...n the system prior to the analytical column and test for front end resolution after every system change 5 4 Spurious Peaks A The column may be contaminated If the samples contain an appreciable level...

Page 31: ...Regenerating Suppressor SRS to the detector conductivity cell at the suppressor end of the line C Install a 10 32 Luer adaptor fitting with a plastic syringe in the ELUENT OUT port of the Self Regene...

Page 32: ...n Suppressed Conductivity ASRS ULTRA AutoSuppression External Water Mode with 10mN Sulfuric Acid Range 10 SFS Background Conductivity 3 15 S Injection Volume 10 L Peak Information Found Components Pea...

Page 33: ...n Suppressed Conductivity ASRS ULTRA AutoSuppression External Water Mode with 10 mN Sulfuric Acid Range 10 SFS Background Conductivity 3 15 S Injection Volume 10 L Peak Information Found Components Pe...

Page 34: ...lush the column for a minimum of 10 minutes with the storage solution Cap both ends securely using the plugs supplied with the column B 4 Column Cleanup The following column cleanup protocols have bee...

Page 35: ...umn Cleanup Procedure A Prepare a 500 mL solution of the appropriate cleanup solution using the guidelines in Section B 4 1 Choosing the Appropriate Cleanup Solution B Disconnect the Suppressor from t...

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