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Atlas Suppressor Manual Document No. 031770-04 Page 1 of 30
ATLAS SUPPRESSOR MANUAL
Anion Atlas® Electrolytic Suppressor(AAES, P/N 056116)
Cation Atlas® Electrolytic Suppressor(CAES, P/N 056118)
©Dionex Corporation, 2004Document No. 031770
Revision 0415 August 2004
Atlas Suppressor Manual Document No. 031770-04 Page 2 of 30
TABLE OF CONTENTS
SECTION 1. INTRODUCTION ........................................................................................................ 4
1.1 Atlas Electrolytic Suppressor System .............................................................................................................. 4
1.2 The Anion Atlas Electrolytic Suppressor (AAES) Electrode, Membrane and MonoDisc Assembly ............... 5
1.3 The Cation Atlas Electrolytic Suppressor (CAES) Electrode, Membrane and MonoDisc Assembly .............. 6
1.4 Modes of Operation ............................................................................................................................................ 71.4.1 The AutoSuppression Recycle Mode ...................................................................................................... 71.4.2 The AutoSuppression External Water Mode ............................................................................................ 81.4.3 Selecting the Correct Suppressor and Mode of Operation ....................................................................... 9
SECTION 2. INSTALLATION ........................................................................................................ 11
2.1 System Requirements ....................................................................................................................................... 11
2.2 Installing the Atlas Electrolytic Suppressor (AES) ......................................................................................... 11
2.3 Gas Separator Waste Tube for Atlas Electrolytic Suppressor (AES) ............................................................. 12
SECTION 3. OPERATION .............................................................................................................. 13
3.1 Chemical Purity Requirements ...................................................................................................................... 133.1.1 Inorganic Chemicals ................................................................................................................................ 133.1.2 Deionized Water ...................................................................................................................................... 133.1.3 Organic Solvents ..................................................................................................................................... 13
3.2 AutoSuppression Recycle Mode Operation .................................................................................................... 143.2.1 Connections ............................................................................................................................................ 153.2.2 Operating the Atlas Electrolytic Suppressor (AES) in the AutoSuppression Recycle Mode ................. 16
3.3 AutoSuppression External Water Mode Operation ........................................................................................ 183.3.1 Connections ............................................................................................................................................ 183.3.2 Regenerant Flow Path Connections in External Water Mode with Pressurized Water Delivery System 193.3.3 Operating AES in the AutoSuppression External Water Mode ............................................................... 20
3.4 Electrolytic Regeneration of Atlas Electrolytic Suppressors ........................................................................ 21
3.5 Storage of Atlas Electrolytic Suppressors (AES) ........................................................................................... 22
Atlas Suppressor Manual Document No. 031770-04 Page 3 of 30
SECTION 4. TROUBLESHOOTING ............................................................................................. 23
4.1 Atlas Electrolytic Suppressor Operational Status ......................................................................................... 234.1.1 Alarm State for Detectors ........................................................................................................................ 23
4.2 High Background Conductivity ....................................................................................................................... 244.2.1 No Current is Applied to the Suppressor or the Set Suppressor Current is too Low .............................. 244.2.2 The Eluent is not Prepared Properly for the Target Application .............................................................. 244.2.3 No Eluent Flows Out of the AES ELUENT OUT Port .............................................................................. 244.2.4 The Eluent Flow Direction or Regenerant Flow Direction is Inadvertently Reversed ............................. 24
4.3 Noisy Baseline ................................................................................................................................................. 254.3.1 Noise from Bubbles in the Conductivity Cell or Liquid Connecting Tubing ........................................... 25
4.4 Poor Chromatographic Efficiency ................................................................................................................... 264.4.1 Incorrect Liquid Connections to AES ELUENT IN and ELUENT OUT Ports .......................................... 264.3.2 Noise from the Back Pressure Coil for the Conductivity Cell .................................................................. 264.3.3 Noise from a Pump .................................................................................................................................. 264.4.2 Incorrect Liquid Connections in Other System Components .................................................................. 26
4.5 Liquid Leaks .................................................................................................................................................... 27
SECTION 5. ATLAS ELECTROLYTIC SUPPRESSOR CLEANUP ............................................ 28
5.1 The Anion Atlas Electrolytic Suppressor (AAES) Cleanup ............................................................................ 285.1.1 Metal Contaminants or Precipitates ........................................................................................................ 285.1.2 Organic Contaminants ............................................................................................................................. 28
5.2 The Cation Atlas Electrolytic Suppressor (CAES) Cleanup .......................................................................... 295.2.1 Organic Contaminants ............................................................................................................................. 29
APPENDIX A - BACK PRESSURE COIL PRESSURE CHECK .................................................. 30
ATTACHMENT 1 - QUICKSTART (Document Number 031771)
Atlas Suppressor Manual Document No. 031770-04 Page 4 of 30
SECTION 1. INTRODUCTION
Figure 1The Atlas Electrolytic Suppression System
The Atlas® Electrolytic Suppressors (AES) are continuous electrolytically regenerated suppressors based on theMonoDiscTM suppression technology developed by Dionex Corporation. As shown in Figure 1, the (AES) systemconsists of the following:
a. An AESb. A Suppressor Control Module or Detector: (Not shown in Figure 1) Examples follow:
Control Module DetectorICS-2000 ED50ARFC CD25ASC-20 IC25A
c. Back Pressure Coilsd. Gas Separator Waste Tube
The AES can be used for most Ion Chromatography (IC) applications using either carbonate or MSA eluents, andhave a maximum suppression capacity of 25 mN eluent at 1.0 mL/min. AES have one suppression bed dimension (4-mm i.d. x 10-mm length) and can be used for 4-, 3-, and 2-mm i.d. column applications. The AES are typically operatedin the recycle mode. For recommended applications see Section 1.4.3. The AES offer improved performance in termsof lower baseline noise, faster start-up, ruggedness, and reliability.
1.1 Atlas Electrolytic Suppressor System
Atlas Suppressor Manual Document No. 031770-04 Page 5 of 30
As shown in Figure 2a, the AAES consists of an anode chamber, a cathode chamber, and an eluent suppression bedchamber separated by cation exchange membranes. The AES has an internal pathway connecting the anode chamber andthe cathode chamber. The MonoDisc suppression bed of the AAES has a dimension of 4-mm i.d. x 10 mm long andconsists of six cation exchange monolith discs and five flow distributors. The monolith discs and flow distributors arealternately sandwiched between the cation exchange membranes that separate the eluent suppression chamber from theanode and cathode regenerant chambers of the suppressor.
The cation exchange monolith discs, in the eluent chamber of the AAES, are porous polyethylene discs that are graftedwith sulfonated functional groups. The flow distributors are impermeable to the liquid flow, except through the small holescut out near their perimeters. The placement of these flow distributors is such that a serpentine flow pathway is created toincrease the effective residence time of the eluent in the suppression bed. As a consequence, the current efficiency andthe dynamic suppression capacity of the suppressor are increased. Because these flow distributors are ion exchangematerials, there is still the transmembrane migration of ions in the suppressor bed due to the electrical field.
When operating the AAES, an appropriate amount of DC current is applied to the suppressor. The water regenerantundergoes electrolysis to form hydroxide ions and hydrogen gas in the cathode chamber while hydronium ions andoxygen gas are formed in the anode chamber. Cation exchange membranes allow hydronium ions to move from the anodechamber into the eluent suppression bed chamber to neutralize hydroxide or carbonate ions in the incoming eluent. Soluteanions are converted to the acid form. Sodium ions in the eluent are attracted to the negativelycharged cathode, stoichiometrically migrate across the cation exchange membranes into the cathode chamber to combinewith hydroxide ions before exiting the suppressor.
Figure 2aAnion Atlas Electrolytic Suppressor (AAES) Electrode, Membrane and MonoDisc Assembly
1.2 The Anion Atlas Electrolytic Suppressor (AAES) Electrode, Membrane and MonoDisc
Eluent In Cation-ExchangeMonolith Disc
Cation-Exchange Flow Distributor Membrane
Eluent OutRegen Out Regen In
AnodeCathode
Cation-Exchange Membrane
Cation-Exchange Membrane
Eluent In Cation-ExchangeMonolith Disc
Cation-Exchange Flow Distributor Membrane
Eluent OutRegen Out Regen In
AnodeCathode
Cation-Exchange Membrane
Cation-Exchange Membrane
Atlas Suppressor Manual Document No. 031770-04 Page 6 of 30
As shown in Figure 2b, the CAES consists of an anode chamber, a cathode chamber, and an eluent suppression bedchamber separated by anion exchange membranes. The CAES has an internal pathway connecting the anode chamber andthe cathode chamber. The MonoDisc suppression bed of the Atlas suppressor has a dimension of 4-mm i.d. x 10 mm longand consists of six anion exchange monolith discs and five flow distributors. The monolith discs and flow distributors arealternately sandwiched between the anion exchange membranes that separate the eluent suppression chamber from theanode and cathode regenerant chambers of the suppressor.
The anion exchange monolith discs in the eluent chamber of the CAES are porous polyethylene discs that are grafted withaminated functional groups. The flow distributors are impermeable to the liquid flow except through the small holes cutout near their perimeters. The placement of these membranes is such that a serpentine flow pathway is created to increasethe effective residence time of the eluent in the suppression bed. As a consequence, the current efficiency and thedynamic suppression capacity of the suppressor are increased. Because these flow distributors are ion exchangematerials, there is still the transmembrane migration of ions in the suppressor bed due to the electrical field.
When operating the CAES an appropriate amount of DC current is applied to the suppressor. The water regenerantundergoes electrolysis to form hydroxide ions and hydrogen gas in the cathode chamber while hydronium ions andoxygen gas are formed in the anode chamber. Anion exchange membranes allow hydroxide ions to move from the cathodechamber into the eluent suppression bed chamber to neutralize hydronium ions in the incoming eluent. Solute cations areconverted to the base form. Sulfate or MSA ions in the eluent, attracted to the positively charged anode,stoichiometrically migrate across the anion exchange membranes into the anode chamber to combine with hydronium ionsbefore exiting the suppressor.
Figure 2bCAES Electrode, Membrane, and MonoDisc Assembly
1.3 The Cation Atlas Electrolytic Suppressor (CAES) Electrode, Membrane and MonoDisc
Eluent In Anion-ExchangeMonolith Disc
Anion-Exchange Flow Distributor Membrane
Eluent OutRegen Out Regen In
AnodeCathode
Anion-Exchange Membrane
Anion-Exchange Membrane
Eluent In Anion-ExchangeMonolith Disc
Anion-Exchange Flow Distributor Membrane
Eluent OutRegen Out Regen In
AnodeCathode
Anion-Exchange Membrane
Anion-Exchange Membrane
Atlas Suppressor Manual Document No. 031770-04 Page 7 of 30
1.4 Modes of Operation
The Atlas Electrolytic Suppressor (AES) uses the electrolysis of water as the regenerant to achieve eluent suppression.There are two modes of electrolytic operation. The most common mode of operation is the AutoSuppression® RecycleMode. In this mode of operation, eluent flows from the eluent outlet of the suppressor into the conductivity cell and isthen recycled through the suppressor regenerant chambers (i.e., the cathode chamber and the anode chamber). Thiseliminates the need for an external source of water but restricts the regenerant flow rate to the eluent flow rate. TheAutoSuppression External Water Mode incorporates an external source of deionized water flowing through theregenerant chambers. This requires the installation of a pressurized bottle system or a pump to provide an external sourceof water. With this configuration, the regenerant flow rate is not restricted to the eluent flow rate.
The AutoSuppression Recycle Mode uses the neutralized conductivity cell effluent as the source of water for theregenerant chamber water. This is the preferable method of operation for the AES. The advantage of this mode ofoperation is its simplicity and ease of use. It reliably provides AutoSuppression for recommended suppressedconductivity applications. As the eluent passes through the AES, it is neutralized to its weakly ionized form. Afterpassing through the conductivity cell, the effluent is redirected to the regenerant inlet of the AES, thus supplying itwith a source of water containing minute amounts of diluted analyte. The amount of water flowing through theregenerant chamber is therefore limited to the eluent flow rate. The Atlas Electrolytic Suppressor cannot be used witheluents containing organic solvents. See Section 3.2, “AutoSuppression Recycle Mode,” for complete operationinstructions.
Figure 3The AutoSuppression Recycle Mode Plumbing Diagram
1.4.1 The AutoSuppression Recycle Mode: (Figure 3)
Gas Separator Waste Tube
Injection Valve
Guard Column
1 or 2 Coils Required (See Table 1)
Waste
Signal to Conductivity Detector
10-32 10-32 10-32
REGEN IN
ELUENT IN
ELUENT OUT
REGEN OUT
CELL
Atlas Suppressor Manual Document No. 031770-04 Page 8 of 30
The AutoSuppression External Water Mode is used where dual detection methods, such as post column reactions,are required. This mode uses a constant source of deionized water from a pressurized bottle or a source of deionizedwater that delivers at 1 to 4 mL/min. The amount of water flowing through the regenerant chambers is thereforeindependent of the eluent flow rate. If the system must be plumbed for applications requiring AutoSuppressionExternal Water Mode, remember that any analysis performed using the AutoSuppression Recycle Mode can also beperformed using the AutoSuppression External Water Mode. See Section 3.3, “AutoSuppression External WaterMode Operation,” for complete operation instructions.
Figure 4The AutoSuppression External Water Mode Plumbing Diagram
1.4.2 The AutoSuppression External Water Mode
Atlas Suppressor Manual Document No. 031770-04 Page 9 of 31
1.4.3 Selecting the Correct Suppressor and Mode of Operation
Table 1Suppressor and Mode of Operation
Suppressor Operation Mode
Benefits Equipment
Recycle Ease of Use No extra equipment
Gas Assisted Recycle
Lower noise combined with ease of use
Gas Assisted Kit (P/N 056886) and gas source
External Water Lower noise
Allows use of eluents with < 40% solvent
DI water source with pump or External Regenerant Installation Kit (P/N 038018)
Gas Assisted External Water
Lower noise with less water usage (flow rate 1-2 mL/min)
Allows use of eluents with < 40% solvent
DI water source with pump or External Regenerant Installation Kit (P/N 038018) plus Gas Assisted Kit (P/N 056886) and gas source
SRS® ULTRA II
Chemical Allows use with eluents containing > 40% solvent or HCl and DAP•HCl
Same options as MMS below
Recycle Low noise and ease of use No extra equipment AES®
External Water Allows use with Post Column Reaction methods
DI water source with pump or External Regenerant Installation Kit (P/N 038018)
Displacement Chemical Regeneration
Low noise and ease of use with extended unattended operation
Chemical regeneration with Displacement Chemical Regeneration Kit (P/N 056882 or 056884)
AutoRegen Low noise and ease of use with extended unattended operation
Chemical regeneration with AutoRegen Kit (P/N 039607 or 039608)
MMS® III
Pressurized Bottle Low noise Chemical regeneration with External Regenerant Installation Kit (P/N 038018)
Atlas Suppressor Manual Document No. 031770-04 Page 10 of 31
Table 2Suppressor Selection Based on Eluent for Anion Analysis
Table 3Suppressor Selection Based on Eluent for Cation Analysis
Eluents for Cation Exchange
CSRS ULTRA II
Cation Self-Regenerating Suppressor
CAES
Cation Atlas Electrolytic Suppressor
CMMS® III
Cation MicroMembrane Suppressor
Methanesulfonic Acid (MSA)
Acceptable performance and ease of use.
High Capacity.
Recommended for applications up to 25 µeq/min for good performance and ease of use.
Best noise performance. Improved ease of use with DCR Kit.
Sulfuric Acid Acceptable performance and ease of use.
High Capacity.
Recommended for applications up to 25 µeq/min for good performance and ease of use.
Best noise performance. Improved ease of use with DCR Kit.
HCl, DAP•HCl Can be used in the Chemical Operation Mode.
Not recommended. Recommended for best performance. Improved ease of use with DCR Kit.
With Solvents Not recommended for eluents with > 40 % solvent.
Not recommended. Recommended for best performance. Improved ease of use with DCR Kit.
Eluents for Anion Exchange
ASRS ULTRA II Anion Self-Regenerating Suppressor®
AAES Anion Atlas Electrolytic Suppressor
AMMS® III Anion MicroMembrane Suppressor
Carbonate Acceptable performance and ease of use.
Recommended for good performance and ease of use.
Best noise performance. Improved ease of use with DCR Kit.
HydroxideRecommended for ease of use and acceptable performance. High
Not recommended for applications requiring > 25 µeq/min.
Best noise performance. Improved ease of use with DCR Kit.
Borate gradientsRecommended for ease of use. Acceptable Performance.
Not recommended.Best noise performance. Improved ease of use with DCR Kit.
With solventsNot recommended for eluents with > 40 % solvent.
Not recommended.Recommended for best performance. Improved ease of use with DCR Kit.
Atlas Suppressor Manual Document No. 031770-04 Page 11 of 30
2.1 System Requirements
The Atlas Electrolytic Suppressor (AES) is designed to operate with Dionex Ion Chromatography (IC) systems equippedwith suppressed conductivity detection. The ICS-2500, ICS-2000, ICS-1500, and ICS 1000 are fully capable of controllingthe AES. For users of the DX-600 systems with ED50A/CD25A or DX-300 with IC25A systems, PeakNet 6.2 + ServicePack 2 (PN6.2+SP2) or greater provides full control of Atlas operation. For users of the DX-600 with ED50/CD25, DX-500,DX-320, DX-120, or DX-100 systems, a Dionex RFC-10 or RFC-30 Reagent Free Controller ot Suppressor Control ModuleSC20 (the external power supply module) is required to operate the AES.
CAUTION: Never apply current to the AES without eluent and water regenerant flowing through the AES at thesame time. The application of current without eluent and regenerant flow can lead to a permanent damageto the suppressor. For optimal suppressor performance, always use the recommended amount of currentto the AES whenever eluent is running through the suppressor.
NOTE: To ensure optimal performance of the AES, it is highly recommended that one uses the Chromeleon orPN6.2+SP2 workstation for full and automated control. When writing a new program file, use the wizard toset the current of the Atlas Suppressor.
SECTION 2. INSTALLATION
2.2 Installing the Atlas Electrolytic Suppressor (AES)
The AES is installed in the column compartment of the Chromatography Module after the analytical column and beforethe conductivity detector cell. To the right, on the ICS-2500, ICS-2000, ICS-1500, ICS-1000, DX-600, DX-500, DX-320, DX-120, and DX-100 instruments, the AES mounts on tabs on the component panel, (see the manual for the ChromatographyModule for instalation of the AES).
IC System ATLAS Hardware Control
RequirementsATLAS Software Control
Requirements
DX-600 or BioLC with ED50A or CD25A detector
DX-600 or BioLC with ED50 or CD25 RFC-10 or RFC 30 Reagent-Free detector Controller DX-500 with ED40/50 or CD20/25 RFC-10 or RFC 30 Reagent-Free detector Controller
RFC-10 or RFC 30 Reagent-Free Controller RFC-10 or RFC 30 Reagent-Free Controller
ICS-1000, ICS-1500, ICS-2000, ICS-2500
DX-320 with IC25A detector Chromeleon/PeakNet 6.2 or higher
Integrated, no additional hardware required
Integrated, no additional hardware required
Integrated, no additional hardware required
CHART A. SYSTEM CONTROL OF ATLAS ELECTROLYTIC SUPPRESSORS
1 Chromeleon or PeakNet can be used to control the DX system
No software required for RFC1
No software required for RFC1
No software required for RFC1
No software required for RFC1
DX-320 with IC25 detector
DX-120
Chromeleon/PeakNet 6.2 or higher
Chromeleon/PeakNet 6.2 or higher
Atlas Suppressor Manual Document No. 031770-04 Page 12 of 30
2.3 Gas Separator Waste Tube for Atlas Electrolytic Suppressor (AES)
The Gas Separator Waste Tube (P/N 045460) is an integral part of the AES system. Its function is to ensure the separationof any hydrogen gas generated in the suppressor during the electrolytic process. The Gas Separator Waste Tube is usedto avoid concentrating the gas in the waste container. The Gas Separator Waste Tube, and required fittings, are shippedin the ICS, RFC, ED50A, CD25A, DX-120 and SC-20 Ship Kits.
CAUTION: DO NOT CAP THE WASTE RESERVOIR! The very small amount of hydrogen gas generated by the AESis not dangerous unless the gas is trapped in a closed container and allowed to concentrate. To operate properly, the GasSeparator Waste Tube must be open to the atmosphere and not in a confined space.
2.3.1. Assemble and install the Gas Separator Waste Tube and waste line following the steps below:
a. Use one or two couplers (P/N 045463) to connect two or three lengths of 1/2" i.d. black polyethylenetubing (P/N 045462) depending of the depth of your waste container.
b. The top of the Waste Separator Tube must extend above the top of the waste container as shown inFigure 5.
c. Place the Gas Separator Waste Tube with the 1/8" o.d. tubing attached into the waste container.
1. Ensure that the bottom of the Gas Separator Waste Tube is resting on the bottom of the wastecontainer, the top of the device (where the white 1/8" o.d. tubing meets the black 1/2" o.d. tubing) isabove the top of the container and that the Gas Separator Waste Tube and the waste container areopen to the atmosphere as shown in Figure 5.
Figure 5Configuration of the Pressurized Water Reservoir and the Gas Separator Waste Tube with the AES
Atlas Suppressor Manual Document No. 031770-04 Page 13 of 30
3.1 Chemical Purity Requirements
Obtaining precise and accurate results requires eluents that are free of ionic impurities. Chemicals and deionized waterused to prepare eluents must be of the purities described below. Low trace impurities and low particulate levels in eluentsand regenerants also help protect your AES and system components from contamination. Dionex cannot guaranteeproper AES performance when the quality of the chemicals and water used to prepare eluents has been compromised.
3.1.1 Inorganic Chemicals
Reagent Grade inorganic chemicals should always be used to prepare ionic eluents. Whenever possible, inorganicchemicals that meet or surpass the latest American Chemical Society standard for purity, a universally acceptedstandard for reagents, should be used. These inorganic chemicals will detail the purity by having an actual lotanalysis on each label.
3.1.2 Deionized Water
The deionized (DI) water used to prepare eluents should be degassed Type I Reagent Grade Water with a specificresistance of 18.2 megohm-cm. The water used for the AutoSuppression External Water Mode should have a specificresistance of 18.2 megohm-cm. The DI water should be free of ionized impurities, organics, microorganisms andparticulate matter larger than 0.2 µm. Filter eluents through a 0.2 µm filter. Bottled HPLC-Grade Water should not beused since most bottled water contains an unacceptable level of ionic impurities. Finally, thoroughly degas allDI water prior to preparing any eluents or regenerants.
3.1.3 Organic Solvents
The AES are currently designed for separations using aqueous eluents only. The AES is not recommended forapplications using solvents. For applications using eluents containing organic solvents, use the Self-RegeneratingSuppressor (SRS ULTRA) or the MicroMembrane Suppressor (MMS III). For suppressor recommendations whenusing solvent in your applications see Tables 2, “Suppressor Selection Based on Eluent for Anion Analysis,” andTable 3, “Suppressor Selection Based on Eluent for Cation Analysis,” .
SECTION 3. OPERATION
This section provides instructions for the start-up and operation of the Atlas Electrolytic Suppressor (AES).
Atlas Suppressor Manual Document No. 031770-04 Page 14 of 30
3.2 AutoSuppression Recycle Mode Operation
The AutoSuppression Recycle Mode is the most convenient AES mode of operation. As shown in Figure 6, the eluentpasses through the suppressor, it is neutralized to produce its weakly ionized form. After passing through theconductivity cell, this effluent is redirected to the regenerant inlet on the suppressor, thus supplying it with a source ofwater containing a small amount of diluted analyte. The main advantage of this mode is its simplicity and ease of use. It isnot necessary to have an external supply of water available for the suppressor.
Gas Separator Waste Tube
Injection Valve
Guard Column
1 or 2 Coils Required (See Table 1)
Waste
Signal to Conductivity Detector
10-32 10-32 10-32
REGEN IN
ELUENT IN
ELUENT OUT
REGEN OUT
Figure 6The AutoSuppression Recycle Mode Plumbing Diagram
CELL
Atlas Suppressor Manual Document No. 031770-04 Page 15 of 30
a. Install the AES in the first slot inside theChromatography Module, as shown in theappropriate Chromatography Module Manual.
b. Connect the outlet of the analytical column tothe ELUENT IN of the AES.
c. Connect the ELUENT OUT port of the AES tothe inlet of the conductivity cell.
d. Connect the back pressure coil(s) between theCELL EXIT port and the REGEN IN port.
e. Install the correct backpressure coil(s) suppliedwith the detector according to table 4.
NOTE: The red back pressure coil(s).(Dionex P/N 45878) are PEEKtubing of 1/16-inch and0.005-inch i.d. Make surethat each red backpressure coilyields about 40-50 psi presuredrop at the flow rate of 1.0 mL/min.by completing the test described inAppendix B.
3.2.1 Connections: (Figure 7 and 8)
Depending on the specific components (analytical column, conductivity cell, back pressure coils) in the system, 1/4-28 or 10-32 ferrule/bolt liquid lines may be required. To purchase or assemble 1/4-28 or 10-32 ferrule/bolt liquid lines,refer to, “Dionex Liquid Line Fittings.” Properly cut tubing to minimize efficiency loss.
CAUTION: As shown in figure 7, The ELUENT IN andELUENT OUT ports, of the Atlas ElectrolyticSuppressor, are deeper than the standard10-32 ports. To ensure minimal band broadeningand optimal chromatographic efficiency, it isextremely critical to make sure that there is nogap between the end of the tubing and thebottom of the port. Hold the tubing in place asthe bolt is tightened.
IMPORTANT NOTE: To avoid adding dead volume to the system, make the length of all eluent lines as short as practically possible.
Gas Separator Waste Tube
Injection Valve
Guard Column
1 or 2 Coils Required (See Table 1)
Waste
Signal to Conductivity Detector
10-32 10-32 10-32
REGEN IN
ELUENT IN
ELUENT OUT
REGEN OUT
Figure 8The AutoSuppression Recycle Mode Plumbing Diagram
Figure 7
CELL
Atlas Suppressor Manual Document No. 031770-04 Page 16 of 30
g. Upon completing all the liquid connections, connect the power supply cable of the Atlas ElectrolyticSuppressor to the appropriate suppressor controller, (i.e. ICS, RFC, SC20, CD25A, ED50A, or IC25A).
CAUTION: The AES must be operated with the Gas Separator Waste Tube (P/N 045460). See Section 2.5, “GasSeparator Waste Tube for Atlas Electrolytic Suppressor.”
f. Small gas bubbles may be trapped inside the liquid line and the conductivity cell, and cause increasedchromatographic baseline noise. To minimize the possibility of encountering this problem, degas the liquidlines by completing the following steps:
1. Disconnect the back pressure coil(s) from thesuppressor REGEN IN port.
2. Turn the pump on.
3. As per Figure 9, Create a pressure differencemomentarily by plugging and unplugging theoutlet of the tubing with the tip of your finger.
4. Repeat the task 2–3 times.
5. Turn your pump off.
6. Reconnect the back pressure coil(s) to theREGEN IN port of the suppressor. Figure 9
Plug the DS3 cell outletwith your finger for 2–3 seconds.
3.2.2 Operating the Atlas Electrolytic Suppressor (AES) in the AutoSuppression Recycle Mode
The AES uses water as the regenerant and has the ability to provide continuous suppression. In theAutoSuppression Recycle Mode, the eluent leaving the conductivity cell is recycled through the regenerantchambers as the water supply. This eliminates the need for an external regenerant water supply. When the AES isoperating in this mode, the amount of water flowing through the regenerant chambers is limited to the eluent flowrate. The AES cannot be used with eluents containing organic solvents.
AESs are designed to have a Maximum Suppression Capacity of 25 mN eluent at 1.0 mL/min. The MaximumSuppression Capacity (MSC) can be calculated using the following equation:
MSC [mN*mL/min]= Eluent Conc. [mN] x Flow Rate [mL/min]
where the eluent concentration should be less or equal to 25 mN.
For optimal suppressor performance, it is important to use the recommended suppressor currents for the targetapplications. For users of a Dionex chromatography system equipped with Chromeleon software. The software willguide you to set the recommended current for the Atlas Electrolytic Suppressor through its interactive Wizard. TheWizard will supply a recommended current based on the inputs for the eluent concentration and the flow rate. (Seethe Wizard Chromeleon Help Screen or Chromeleon user instructions for details). The Chromeleon software willautomatically enter the recommended current into the program file and will apply that current to the Atlas ElectrolyticSuppressor. Dionex strongly recommends using the Wizard to set the current to the Atlas Suppressor when writingnew program files.
If a Dionex RFC-30, RFC-10, or SC20 module is used as the power supply for the AES, the recommended currentshould be manually set according to the appropriate module operation instructions. The following table summarizesthe anion and cation separation columns compatible with the AES, standard eluents and flow rates used with thesecolumns, and the recommended currents for the AES.
Atlas Suppressor Manual Document No. 031770-04 Page 17 of 30
Table 5Recommended Operating Currents for Atlas Suppressors in Recycle Mode
Column Eluent Flow Rate, mL/min Current, mA
AS4A-SC 4-mm 1.8 mM Na2CO3/1.7 mM NaHCO3 2.00 35
AS4A-SC 2-mm 1.8 mM Na2CO3/1.7 mM NaHCO3 0.50 9
AS9-HC 4-mm 9.0 mM Na2CO3 1.00 58
AS9-HC 2-mm 9.0 mM Na2CO3 0.25 15
AS12A 4-mm 2.7 mM Na2CO3/0.3 mM NaHCO3 1.50 28
AS12A 2-mm 2.7 mM Na2CO3/0.3 mM NaHCO3 0.38 7
AS14 4-mm 3.5 mM Na2CO3/1.0 mM NaHCO3 1.20 31
AS14 2-mm 3.5 mM Na2CO3/1.0 mM NaHCO3 0.30 8
AS14A 3-mm 8.0 mM Na2CO3/1.0 mM NaHCO3 0.50 28
CS12A 4-mm 22 mM MSA 1.00 71
CS12A-5µm 3-mm 20 mM MSA 0.50 33
CS12A 2-mm 22 mM MSA 0.25 18
CS14 4-mm 10 mM MSA 1.00 33
CS14 2-mm 10 mM MSA 0.25 9
For other column and eluent conditions, the recommended current for the Atlas Electrolytic Suppressors should becalculated using the following equation:
Current (mA) = 3.22 x [eluent, mN] x [flow rate, mL/min]For anion separations:
[eluent, mN] = 2 x [CO3-2, mM] + [HCO3
-, mM] + [OH-, mM]For cation separations:
[eluent, mN] = 2 x [H2SO4, mM] + [MSA, mM]
To ensure the optimal performance of the Atlas Electrolytic Suppressors, avoid applying excess current to thesuppressors. Excess operation currents lead to excess heat generation, which can reduce the suppressor lifetime andcause higher chromatographic baseline noise. The maximum operating current for the Atlas Electrolytic Suppressorcan be calculated using the following equation:
Maximum Current [mA] = Flow Rate [ mL/min] x 100
For example, the maximum current is 100 mA at the flow rate of 1.0 mL/min, 50 mA at the flow rate of 0.5 mL/min, or 25mA at the flow rate of 0.25 mL/min. The overriding maximum current is 100 mA. Once the recommended suppressorcurrent is determined, turn on the pump flow rate, apply the recommended current to the suppressor, and start tooperate the ion chromatography system.
NOTE: Make sure to turn off the power to the RFC-30, RFC-10, or SC20 module (the stand-alone power supplyto the Atlas Electrolytic Suppressor) when you prime the pump in the chromatography system.Otherwise, the suppressor can be damaged because the eluent is not flowing through the suppressorwhile the electrical current is applied. When using PeakNet control, the suppressor will automaticallyshut off when the eluent flow is zero.
Atlas Suppressor Manual Document No. 031770-04 Page 18 of 30
3.3 AutoSuppression External Water Mode Operation
Any analysis that can be performed using the AutoSuppression Recycle Mode can also be done using theAutoSuppression External Water Mode. The AutoSuppression External Water Mode is used where dual detectionmethods, such as post column reactions, are required. A constant source of deionized water having a specific resistanceof 10 megohm or greater, is supplied to the regenerant chambers to generate ions for neutralization.
Figure 12The AutoSuppression External Water Mode Plumbing Diagram
3.3.1 Connections: (Figure 11 and 12)
Depending on the specific components (analytical column, conductivity cell, back pressure coils) in the system, 1/4-28 or 10-32 ferrule/bolt liquid lines may be required. To purchase or assemble 1/4-28 or 10-32 ferrule/bolt liquid lines,refer to, “Dionex Liquid Line Fittings.” Properly cut tubing to minimize efficiency loss.
CAUTION: As shown in figure 11, The ELUENT IN andELUENT OUT ports, of the Atlas ElectrolyticSuppressor, are deeper than the standard10-32 ports. To ensure minimal band broadeningand optimal chromatographic efficiency, it isextremely critical to make sure that there is nogap between the end of the tubing and thebottom of the port. Hold the tubing in place asthe bolt is tightened.
IMPORTANT NOTE: To avoid adding dead volume to the system, make the length of all eluent lines as short as practically possible.
Figure 11
a. Install the AES in the first slot inside theChromatography Module, as shown in theappropriate Chromatography Module Manual.
b. Connect the outlet of the analytical column tothe ELUENT IN of the AES.
c. Connect the ELUENT OUT port of the AES tothe inlet of the conductivity cell.
d. Connect the outlet of the conductivity cell tothe inlet of the back pressure coil(s).
e. Connect the outlet of the back pressure coil(s)to the waste line.
f. Install the correct backpressure coil(s) suppliedwith the detector according to Table 6 and Figure 12.
NOTE: The red back pressure coil(s). (Dionex P/N45878) are PEEK tubing of 1/16-inch and0.005-inch i.d. Make sure that each redbackpressure coil yields about 40-50 psipresure drop at the flow rate of 1.0 mL/min.by completing the test described inAppendix B.
Atlas Suppressor Manual Document No. 031770-04 Page 19 of 30
f. Small gas bubbles may be trapped inside the liquid line and the conductivity cell, and cause increasedchromatographic baseline noise. To minimize the possibility of encountering this problem, degas the liquidlines by completing the following steps:
1. Disconnect the back pressure coil(s) from thesuppressor REGEN IN port.
2. Turn the pump on.
3. As per Figure 13, Create a pressure differencemomentarily by plugging and unplugging theoutlet of the tubing with the tip of your finger.
4. Repeat the task 2–3 times.
5. Turn your pump off.
6. Reconnect the back pressure coil(s) to theREGEN IN port of the suppressor.
g. Upon completing all the liquid connections, connect the power supply cable of the Atlas ElectrolyticSuppressor to the appropriate suppressor controller, (i.e. ICS, RFC, SC20, CD25A, ED50A, or IC25A).
CAUTION: The AES must be operated with the Gas Separator Waste Tube (P/N 045460). See Section 2.5, “GasSeparator Waste Tube for Atlas Electrolytic Suppressor.”
Figure 13Plug the DS3 cell outlet
with your finger for 2–3 seconds.
3.3.2 Regenerant Flow Path Connections in External Water Mode with Pressurized Water DeliverySystem (Figure 12)
The External Regenerant Installation Kit (P/N 038018) contains all of the components needed to install and operatethe AES with a pressurized water reservoir. The kit contains the SRS Installation Parts Kit (P/N 039055) applicable toAtlas, a 25 psi regulator (P/N 038201) and a 4-liter water reservoir (P/N 039164).
a. Make the following air line connections:1. Locate the pieces of tinted 1/8" o.d. plastic tubing (P/N 030089) supplied in the Suppressor
Installation Parts Kit.2. Push the end of one piece of 1/8" o.d. tubing over the barbed fitting of the regulator.3. Connect the other end of the tubing to the source of air pressure.4. Push one end of the second piece of 1/8" o.d. tubing over the other barbed fitting of the regulator.5. Push the other end of this tubing over the barbed fitting (P/N 030077) in the pressure inlet of the
plastic reservoir.b. Make the following water line connections.
1. Use a coupler (P/N 039056) to connect one end of the 30" tubing assembly (P/N 035727) that comes inthe Installation Kit to the water reservoir.
2. Connect the other end of this tubing to the REGEN IN port of the Atlas Electrolytic Suppressor.3. Using a coupler (P/N 039056) and a 1/8" o.d. piece of tubing (P/N 035728) from the Installation Kit,
connect one end of this line to the REGEN OUT port of the AES4. Connect the other end of the line to the Gas Separator Waste Tube.
c. Fill the water source reservoir.d. Make sure that the O-ring is inside the cap of the reservoir before screwing the cap onto the reservoir.e. Screw the cap onto the reservoir tightlyf. Place the reservoir near the Chromatography Module.d. With no current applied, adjust the external water flow rate to approximately 1–2 mL/min .
NOTE: A safety relief valve on the reservoir regulator prevents pressure greater than 25 psi from being appliedto the water reservoir.
Atlas Suppressor Manual Document No. 031770-04 Page 20 of 30
3.3.3 Operating AES in the AutoSuppression External Water Mode
The AES uses water as the regenerant and has the ability to provide continuous suppression. The AutoSuppressionExternal Water Mode requires an external source of deionized water for the regenerant chambers. When the AES isoperating in this mode, the amount of water flowing through the regenerant chambers is independent of the eluentflow rate.
Atlas Electrolytic Suppressors are designed to have a maximum suppression capacity of 25 mN eluent at 1.0 mL/min.The maximum suppression capacity (MSC) can be calculated using the following equation:
MSC [mN*mL/min]= Eluent Conc. [mN] x Flow Rate [mL/min]
where the eluent concentration should be less or equal to 25 mN.
For optimal suppressor performance, it is important to use the recommended suppressor currents for the targetapplications. For users of a Dionex chromatography system equipped with Chromeleon software. The software willguide you to set the recommended current for the Atlas Electrolytic Suppressor through its interactive Wizard. TheWizard will supply a recommended current based on the inputs for the eluent concentration and the flow rate. See theWizard Chromeleon Help Screen or Chromeleon user instructions for details. The Chromeleon software willautomatically enter the recommended current into the program file and will apply that current to the Atlas ElectrolyticSuppressor. Dionex strongly recommends using the Wizard to set the current to the Atlas Suppressor when writingnew program files.
If a Dionex RFC module is used as the power supply for the Atlas Electrolytic Suppressor, the recommended currentshould be manually set according to the RFC module operation instructions. The following table summarizes thetypical anion and cation separation columns compatible with the Atlas Electrolytic Suppressor, standard eluents andflow rates used with these columns, and the recommended currents for the Atlas Electrolytic Suppressors.
Table 7Recommended Operating Currents for Atlas Suppressors in External Water Mode
Column Eluent Flow Rate, mL/min Current, mA
AS4A-SC 4-mm 1.8 mM Na2CO3/1.7 mM NaHCO3 2.00 35
AS4A-SC 2-mm 1.8 mM Na2CO3/1.7 mM NaHCO3 0.50 9
AS9-HC 4-mm 9.0 mM Na2CO3 1.00 58
AS9-HC 2-mm 9.0 mM Na2CO3 0.25 15
AS12A 4-mm 2.7 mM Na2CO3/0.3 mM NaHCO3 1.50 28
AS12A 2-mm 2.7 mM Na2CO3/0.3 mM NaHCO3 0.38 7
AS14 4-mm 3.5 mM Na2CO3/1.0 mM NaHCO3 1.20 31
AS14 2-mm 3.5 mM Na2CO3/1.0 mM NaHCO3 0.30 8
AS14A 3-mm 8.0 mM Na2CO3/1.0 mM NaHCO3 0.5 28
CS12A 4-mm 22 mM MSA 1.00 71
CS12A-5µm 3-mm 20 mM MSA 0.50 33
CS12A 2-mm 22 mM MSA 0.25 18
CS14 4-mm 10 mM MSA 1.00 33
CS14 2-mm 10 mM MSA 0.25 9
Atlas Suppressor Manual Document No. 031770-04 Page 21 of 30
For other column and eluent conditions, the recommended current for the Atlas Electrolytic Suppressors (AES)should be calculated using the following equation:
Current (mA) = 3.22 x [eluent, mN] x [flow rate, mL/min]
For anion separations:[eluent, mN] = 2 x [CO3
-2, mM] + [HCO3-, mM] + [OH-, mM]
For cation separations:[eluent, mN] = 2 x [H2SO4, mM] + [MSA, mM]
To ensure the optimal performance of the AES, avoid applying excess current to the suppressors. Excess operationcurrents lead to excess heat generation, which can reduce the suppressor lifetime and cause higher chromatographicbaseline noise. The maximum operating current for the AES can be calculated using the following equation:
Maximum Current [mA] = Flow Rate [ mL/min] x 100
For example, the maximum current is 100 mA at the flow rate of 1.0 mL/min, 50 mA at the flow rate of 0.5 mL/min, or 25mA at the flow rate of 0.25 mL/min. The allowed maximum current is 100 mA. Once the recommended suppressorcurrent is determined, turn on the pump flow rate, apply the recommended current to the suppressor, and start tooperate the ion chromatography system.
NOTE: Make sure to turn off the power to the RFC-30 or RFC-10 module (the stand-alone power supply tothe AES whenyou prime the pump in the chromatography system. Otherwise, the suppressor can bedamaged because the eluent is not flowing through the suppressor while the electrical current isapplied. When using PeakNet control, the suppressor will automatically shut off when the eluent flowis zero.
3.4 Electrolytic Regeneration of Atlas Electrolytic Suppressors
For proper operation of the Atlas Electrolytic Suppressor and the associated ion chromatographic system, apply theappropriate amount of current to the Atlas Electrolytic Suppressor when eluent is flowing through the suppressor. Failureto apply the appropriate amount of current to the AES when eluent is flowing through the suppressor leads to theexhaustion of the suppressor. The most common symptom associated with the exhausted suppressor is high detectorbackground conductance. When the AES suppressor becomes exhausted, the suppressor must be regenerated to restoreits performance. The procedure for the electrolytic regeneration of AES suppressors is given below.
a. Determine the appropriate current required for the electrolytic regeneration based on the eluent flow rate usedaccording to the following equation:
Regeneration Current [mA] = Flow Rate [ mL/min] x 100.For example, the regeneration current is 100 mA at the flow rate of 1.0 mL/min, 50 mA at the flow rate of 0.5 mL/min, or 25 mA at the flow rate of 0.25 mL/min. Use the regeneration current of 100 mA if the eluent flow rate isgreater than 1.0 mL/min.
b. Make sure that the eluent flow is on.
c. Apply the regeneration current determined in Step 1 to the AES suppressor for 60 minutes to regenerate thesuppressor.
d. Reset the suppressor current to the recommended current value for normal AES operation under the eluentconditions used.
e. Resume normal system operation.
Atlas Suppressor Manual Document No. 031770-04 Page 22 of 30
3.5 Storage of Atlas Electrolytic Suppressors (AES)
The AES is shipped with an aqueous eluent as the storage solution. If the suppressor will not be used for more than oneweek, prepare it for storage according to the following steps.
a. Use a 3-mL or 5-mL disposable plastic syringe to push approximately 3 mL each of deionized water through theELUENT IN port and REGEN IN port of the suppressor, respectively.
b. Plug all eluent and regen ports.
c. To resume operation, connect the suppressor to the system, and allow the system to equilibrate before startinganalysis.
The ion exchange monoliths and membranes in the AES must be completely hydrated to maintain the AES performance.Make sure to follow the above steps when the AES Suppressor is removed (uninstalled) from the chromatographicsystem.
Atlas Suppressor Manual Document No. 031770-04 Page 23 of 30
4.1.1 Alarm State for Detectors
Detector modules in IC systems equipped with Chromeleon software provide full operation control to AESs. Whenusing these modules, the suppressor type and current setting will be shown on the module front panel and recordedin the Chromeleon control panel audit trail window.
ERROR MESSAGES:a. Open circuits are detected from the suppressor: This may be caused if:
1. The wrong suppressor is being used.2. The suppressor is damaged.
b. Please check and ensure the correct suppressor is connected: This is displayed if:1. The SRS cable is not connected properly to the AES.2. The wrong suppressor type is selected.3. The AES suppressor is damaged.
To prevent an alarm state, make sure that:1. The SRS cable is connected properly to the AES suppressor.2. The correct suppressor type is selected.3. The eluent flow is on.
If the problem persists, it is possible that the AES suppressor is damaged.
SECTION 4. TROUBLESHOOTING
The purpose of the Troubleshooting Guide is to help solve operating problems that may arise while using the AtlasElectrolytic Suppressor (AES). For more information on problems that originate with the Ion Chromatograph (IC) or thespecific separation column, refer to the Troubleshooting Guide in the appropriate Installation Manual. If you cannot solve theproblem on your own, contact the Dionex Regional Office nearest you (see, “Dionex Worldwide Offices”).
Observation Possible Problem See Section
Atlas Electrolytic Suppressor Operational Error Message 4.1
Alarm State for Detectors 4.1.1
High Background Conductivity 4.2
No Current is Applied to the Suppressor or the Set Suppressor Current is too Low 4.2.1
The Eluent is not Prepared Properly for the Target Application 4.2.2
No Eluent Flows Out of the AES ELUENT OUT Port. 4.2.3
The Eluent Flow Direction or Regenerant Flow Direction is Inadvertently Reversed. 4.2.4
Noisy Baseline 4.3
Noise from Bubbles in the Conductivity Cell or Liquid Connecting Tubing 4.3.1
Noise from the Back Pressure Coil for the Conductivity Cell 4.3.2
Noise from a Pump that is Not Primed Properly 4.3.3
Poor Chromatographic Efficiency 4.4
Incorrect Liquid Connections to AES ELUENT IN and ELUENT OUT Ports 4.4.1
Incorrect Liquid Connections in Other System Components 4.4.2
Liquid Leaks 4.5
4.1 Atlas Electrolytic Suppressor Operational Status
Atlas Suppressor Manual Document No. 031770-04 Page 24 of 30
4.2.1 No Current is Applied to the Suppressor or the Set Suppressor Current is too Low
CHECK THE FOLLOWING:a. The SRS cable is connected properly to the AES suppressor.b. The correct suppressor type is selected.c. The current is applied to the AES suppressor when the eluent flow is on.
If the current is applied to the AES suppressor and the background conductivity remains high, the set current may betoo low for the eluent concentration and flow rate used. For users of Chromeleon, make sure to use the Wizard in thesoftware to determine the appropriate amount of the suppressor current required for the given eluent concentrationand flow rate. For users of RFC-30, RFC-10, or SC20 modules, follow the instructions in Section 3.2.2, “Operating AESin the AutoSuppression Recycle Mode” or Section 3.3.3, “Operating AES in the AutoSuppression External WaterMode” to determine the appropriate amount of the suppressor current required for the given eluent concentrationand flow rate.
4.2.2 The Eluent is not Prepared Properly for the Target Application
If the eluent concentration is higher than that specified for the intended application, the AES may not suppress thehigh concentration using the set current, resulting in high background conductivity. Confirm the eluentconcentration for the intended application. For users of Chromeleon, make sure to use the Wizard in the software todetermine the appropriate amount of the suppressor current required for the given eluent concentration and flow rate.For users of RFC-30, RFC-10, or SC20 modules, follow the instructions in Section 3.2.2, “Operating AES in theAutoSuppression Recycle Mode” or Section 3.3.3, “Operating AES in the AutoSuppression External Water Mode” todetermine the appropriate amount of the suppressor current required for the given eluent concentration and flow rate.
Remake the eluent to be sure that the concentration is correct. Also, make sure that chemicals of the required puritywere used to make the eluent (see Section 3.1, “Chemical Purity Requirements”).
4.2.3 No Eluent Flows Out of the AES ELUENT OUT Port
If there is no flow out of the AES ELUENT OUT port, make sure that eluent is entering the AES suppressor at the ELUENTIN port. If there is no flow at this point, trace the eluent flow path backward through the system to find and remove theblockage.
If there is eluent flow into the AES ELUENT IN port but not out of the ELUENT OUT port, and there are no visible leaksfrom the side seam of the suppressor, a break in the membranes separating the suppressor regenerant chambers from theeluent chamber is probably allowing eluent to leak into the regenerant chambers. If this is the case, then the AES suppressormust be replaced.
4.2.4 The Eluent Flow Direction or Regenerant Flow Direction is Inadvertently Reversed
High background conductivity can be caused by the fact that the eluent flow direction or regenerant flow direction isinadvertently reversed. Make sure that the eluent from the column is correctly connected to the ELUENT IN port of theAES suppressor and the regenerant solution is correctly connected to the REGEN IN port of the AES suppressor.
4.2 High Background Conductivity
There are a number of system and operation errors that can cause high background conductivity when using an AtlasSuppressor. The common errors and the remedial steps are summarized below.
Atlas Suppressor Manual Document No. 031770-04 Page 25 of 30
4.3.1 Noise from Bubbles in the Conductivity Cell or Liquid Connecting Tubing
Small gas bubbles may be introduced and trapped in the conductivity cell or liquid connecting tubing during eitherthe installation of the AES or the normal system operation. The presence of small gas bubbles in the conductivity cellor liquid connecting tubing can produce noisy chromatographic baseline as shown in Figure 14.
Figure 14Noise from Bubbles in the Conductivity Cell or Liquid Connecting Tubing
µS
0 20.0 40.0 60.0 80.0 100.0
Minutes
16.540
16.550
16.560
16.570
16.580
16.590
16.600
16.610
16.620
Cell degas steps A - D are performed here.
µS
0 20.0 40.0 60.0 80.0 100.0
Minutes
16.540
16.550
16.560
16.570
16.580
16.590
16.600
16.610
16.620
µS
0 20.0 40.0 60.0 80.0 100.0
Minutes
16.540
16.550
16.560
16.570
16.580
16.590
16.600
16.610
16.620
Cell degas steps A - D are performed here.
4.3 Noisy Baseline
One major advantage of the Atlas Electrolytic Suppressor (AES) is low chromatographic baseline noise. Therefore, it isimportant that all ion chromatographic (IC) system components are maintained and operated properly. With a properlyoperated system, the chromatographic baseline noise obtained using the AES is typically 2–3 nS or lower. If the systemcomponents are not operating properly, one may experience noisy chromatographic baselines such as shown in Figure 14.
The small gas bubbles in the conductivity cell or liquid connecting tubing can be removed by using the followingprocedure.
a. Disconnect the back pressure coilfrom the suppressor REGEN IN port.
b. Turn the pump on.c. As shown in Figure 15, Create a pressure
difference momentarily (3 to 5 seconds),by plugging and unplugging the outlet ofthe tubing with the tip of your finger.
d. Repeat the task for 2–3 times.e. Turn your pump off and reconnect the
backpressure coil to the REGEN IN portof the suppressor.
Figure 15Plug the DS3 cell outlet
with your finger for 2–3 seconds.
Atlas Suppressor Manual Document No. 031770-04 Page 26 of 30
4.3.2 Noise from the Back Pressure Coil for the Conductivity Cell
The backpressure coil(s) installed at the outlet of the conductivity cell should generate a pressure in the range of20–100 psi at the eluent flow rate used. Higher chromatographic baseline noise may be observed if the back pressurecoil(s) generate a pressure outside of the recommended range. Please follow the instructions in Appendix B, “BackPressure Coil Pressure Check” to determine the pressure drop across the backpressure coil(s) used in the system.
4.3.3 Noise from a Pump
If the pump is not primed properly, small gas bubbles may be trapped inside the pump heads or check valves, whichcan lead to the fluctuation of pump operating pressure and higher chromatographic baseline noise. Make sure thatthe pump is properly primed. Refer to the pump operation manual for the recommended priming procedure.
NOTE: Make sure to turn off the power to the RFC-30, RFC-10, or SC20 module (the stand-alone powersupply to the AES when you prime the pump in the chromatography system. Otherwise, the suppressorcan be damaged because the eluent is not flowing through the suppressor while the electrical current isapplied. When using PeakNet control, the suppressor will automatically shut off when the eluent flowis zero.
4.4 Poor Chromatographic Efficiency
4.4.1 Incorrect Liquid Connections to AES ELUENT IN and ELUENT OUT Ports
Figure 16 showes that the ELUENT IN and ELUENT OUT ports of the AES are deeper than the standard 10-32 ports.Incorrect liquid connections to AES ELUENT IN and ELUENT OUT ports can lead to poor chromatographicefficiency. To ensure minimal band broadening and optimal chromatographic efficiency, it is extremely critical to makesure that there is no gap between the end of the tubing and the bottom of the port. Hold the tubing in place as thebolt is tightened.
Figure 16
4.4.2 Incorrect Liquid Connections in Other System Components
Lower efficiency is expected when using Atlas compared to applications using a 2-mm Self-Regenerating Suppressor(SRS ULTRA) due to the higher internal volume of the Atlas Suppressor.
Incorrect liquid connections in other system components can also cause poor chromatographic efficiency. To ensureminimal band broadening and optimal chromatographic efficiency, it is critical to minimize the length of PEEK tubingused to make liquid connections in the system, and make sure there is no gap between the end of the tubing and thebottom of the connecting ports.
Atlas Suppressor Manual Document No. 031770-04 Page 27 of 30
4.5 Liquid Leaks
The system back pressure downstream from the Atlas Electrolytic Suppressor (AES), should not exceed 100 psi. If thesystem back pressure downstream from the AES is greater than 400 psi, the high system backpressure can cause the AESto leak. Find and eliminate the source of the pressure. The AES suppressor will usually recover from momentaryoverpressure conditions. If the AES suppressor continues to leak when operated within the proper back pressure range, itmust be replaced.
Atlas Suppressor Manual Document No. 031770-04 Page 28 of 30
5.1.1 Metal Contaminants or Precipitates
a. Turn off the power to the AAES.b. Disconnect the analytical column from the injection valve.c. Disconnect the guard column from the AAES. Refer to the specific analytical column Installation
Instructions and Troubleshooting Guide for column cleanup procedures.d. 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.e. Disconnect the liquid line from the AAES ELUENT OUT port to the cell at the cell fitting.f. Reconnect the liquid line from the AAES ELUENT OUT port to the cell at the cell fitting to the REGEN IN
port.g. Connect a temporary line from the priming block or the low-pressure tee on the isocratic or gradient pump
to a container with a solution of 0.5 M oxalic acid.h. Pass 60 mL of this solution through the AAES using the Trap Column / Suppressor Clean-up Kit (P/N
059649) or pump this solution through the AAES at 2.0 mL/min for 30 minutes.
NOTE: Bypassing internal pump manifolds when temporarily pumping high concentration cleaningsolutions significantly reduces the time required to re-equilibrate the system to lowconcentration eluents.
i. Flush the AAES with deionized water at 2 mL/min for 30 minutes.j. Reinstall the AAES according to procedures in Section 3.2.1 (Eluent and Regenerant Flow Path
Connections in the AutoSuppression Recycle Mode Operation), or Section 3.3.1 (Eluent Flow PathConnections in the AutoSuppression External Water Mode Operation), and resume operation.
5.1.2 Organic Contaminants
a. Turn off the power to the AAES.b. Disconnect the analytical column from the injection valve.c. Disconnect the guard column from the AAES. Refer to the specific analytical column Installation
Instructions and Troubleshooting Guide for column cleanup procedures.d. 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. If you are running in theAutoSuppression Recycle Mode, proceed to "e".
e. Disconnect the liquid line from the AAES ELUENT OUT port to the cell at the cell fitting.f. Reconnect the liquid line from the AAES ELUENT OUT port to the cell at the cell fitting to the REGEN IN
port.g. Connect a temporary line from the priming block or the low-pressure tee on the isocratic or gradient pump
to a container with a solution of freshly prepared 10% 1.0 M H2SO4/90% acetonitrile.
NOTE: H2SO4/acetonitrile solutions are not stable during long term storage so this cleanup solutionmust be made immediately before each column cleanup. Alternatively, it can beproportioned from 1 bottle containing 1.0 M H2SO4 and another bottle containing 100%acetonitrile.
h. Pass 60 mL of this solution through the AAES using the Trap Column / Suppressor Clean-up Kit (P/N059649) or pump this solution through the AAES at 2.0 mL/min for 30 minutes.
SECTION 5. ATLAS ELECTROLYTIC SUPPRESSOR CLEANUP
This section describes routine cleanup procedures for the Atlas Electrolytic Suppressors (AES) in the case of contamination.Consult the Troubleshooting Guide, section 4 of this manual, to first determine that the system is operating properly. If theAES is determined to be the source of higher than normal back pressure, higher than anticipated conductivity, decreasedsuppression capacity, or decreased sensitivity, cleaning it may restore the performance of the system. Use the followingprocedures to clean the AES.
5.1 The Anion Atlas Electrolytic Suppressor (AAES) Cleanup
Atlas Suppressor Manual Document No. 031770-04 Page 29 of 30
5.2.1 Organic Contaminants
a. Turn off the power to the CAES.b. Disconnect the analytical column from the injection valve.c. Disconnect the guard column from the CAES. Refer to the specific analytical column Installation
Instructions and Troubleshooting Guide for column cleanup procedures.d. If you are running in the AutoSuppression External Water Mode, turn off the external water and
disconnect the external water line from the CAES REGEN IN port. If you are running in theAutoSuppression Recycle Mode, proceed to "e".
e. Disconnect the liquid line from the CAES ELUENT OUT port to the cell at the cell fitting.f. Reconnect the liquid line from the CAES ELUENT OUT port to the cell at the cell fitting to the REGEN IN
port.e. Connect a temporary line from the priming block or the low-pressure tee on the isocratic or gradient pump to
a container with a solution of freshly prepared 10% 1.0 M MSA/90% acetonitrile.
NOTE: MSA/acetonitrile solutions are not stable during long term storage so this cleanup solutionmust be made immediately before each column cleanup. Alternatively, it can beproportioned from 1 bottle containing 1.0 M MSA and another bottle containing 100%acetonitrile.
h. Pass 60 mL of this solution through the CAES using the Trap Column / Suppressor Clean-up Kit (P/N 059649)or pump this solution through the CAES at 1.0 mL/min for 60 minutes.
NOTE: Bypassing internal pump manifolds when temporarily pumping high concentration cleaningsolutions significantly reduces the time required to re-equilibrate the system to low
i. Flush the CAES with deionized water at 2 mL/min for 30 minutes.j. Reinstall the CAES according to procedures in Section 3.2.1 (Eluent and Regenerant Flow Path
Connections in the AutoSuppression Recycle Mode Operation), or Section 3.3.1 (Eluent Flow PathConnections in the AutoSuppression External Water Mode Operation), and resume operation.
NOTE: Bypassing internal pump manifolds when temporarily pumping high concentration cleaningsolutions significantly reduces the time required to re-equilibrate the system to low
i. Flush the AAES with deionized water at 2 mL/min for 30 minutes.j. Reinstall the AAES according to procedures in Section 3.2.1 (Eluent and Regenerant Flow Path Connections in
the AutoSuppression Recycle Mode Operation), or Section 3.3.1 (Eluent Flow Path Connections in theAutoSuppression External Water Mode Operation), and resume operation.
5.2 The Cation Atlas Electrolytic Suppressor (CAES) Cleanup
Atlas Suppressor Manual Document No. 031770-04 Page 30 of 30
2-mm and 3-mm ChromatographyP/N 045878 (1 Coil)
0.25 mL/min. = 2 red backpressurecoils
0.50 mL/min. = 1 red backpressurecoil
4-mm ChromatographyP/N 045877 (1 Coil)
1.0 mL/min. = 2 black backpressurecoils
2.0 mL/min. = 1 black backpressurecoil
Waste
InjectionValve
Waste
InjectionValve
APPENDIX A - BACK PRESSURE COIL PRESSURE CHECK
Waste
Cell
InjectionValve
Coil #2
Coil #1
Waste
Cell
InjectionValve
Coil #2
Coil #1
A. Disconnect the eluent line from the injection valveto the column at the column inlet and direct it to awaste container. Turn the pump on at yourapplication flow rate. After 2 to 3 minutes ofequilibration record pressure P1.
Back Pressure Coil Pressure Testfor Dionex Suppressors
B. Connect the eluent line from the injection valvedirectly to the detector cell inlet with therecommended number of back pressure coils attachedfor your application (see the table above). Turn thepump on. After 2 to 3 minutes of equilibration recordpressure P2.
C. The correct operating pressure range for thesuppressor being tested is listed to the right. If thepressure falls outside the specified range, perform thesteps below:
1. Repeat steps A and B to verify P1 and P2.2. Check the tubing for restrictions or crimps.3. Remove one of the coils or shorten the length of tubing in the coils so that P2–P1 is in the proper range.
Eluent Line
Eluent Line
Document No. 031759-02 Page 1 of 1 12 February 2001
PressureSuppressor RequirementSRS P2 - P1 < 40 psiAES P2 - P1 = 20 - 100 psiMMS P2 - P1 < 40 psi
For SRS ULTRA and MMS III
For AES, use the RED Back Pressure Coils Only
Document No. 031771-04 Page 1 of 1 26 July 2004
Gas Separator Waste Tube
Injection Valve
Guard Column
1 or 2 Coils Required (See Table 1)
Waste
Signal to Conductivity Detector
10-32 10-32 10-32
REGEN IN
ELUENT IN
ELUENT OUT
REGEN OUT
10-32
1. Hydrating the Suppressor
Use a 3 mL or 5 mL disposable plastic syringe to push approximately 3 mL of deionized water through the ELUENT IN port and REGEN IN port of the suppressor (See Figure 1).
P/N Description 016640 5 cc plastic syringe 046888 Fitting, Female Luer Lock 10-32 Threads, Nylon
2. Connecting the AES to the System
Install the AES in your system in the recycle mode according to the liquid connections shown in Figure 1 and ID PEEK liquid line sizes in Table 1.
3. The AES 10-32 Fitting CAUTION: The ELUENT IN and ELUENT OUT ports, of the Atlas Electrolytic Suppressor, are deeper than the standard 10-32 ports. To ensure minimal band broadening and optimal chromatographic efficiency, it is extremely critical to make sure that there is no gap between the end of the tubing and the bottom of the port. Hold the tubing in place as the bolt is tightened (See Figure 2).
A. Install the correct back pressure coil(s) supplied with the chromatography module according to the table above.
B. Small gas bubbles may be trapped inside the liquid line and the conductivity cell causing increased chromatographic baseline noise. To minimize the possibility of encountering this problem; degas the liquid lines by completing the following steps:
1. Disconnect the back pressure coil(s) from the suppressor REGEN IN port. 2. Turn the pump on and create a monetary pressure difference by plugging and unplugging the outlet of the tubing with the tip of your finger. 3. Repeat the task 2–3 times. 4. Turn the pump off and reconnect the back pressure coil(s) to the REGEN IN port of the suppressor.
C. Upon completing all liquid connections, connect the power supply cable of the Atlas Electrolytic Suppressor to the appropriate suppressor controller (i.e., ICS-2000, RFC, SC20, CD25A, ED50A, or IC25A).
NOTE: Read the suppressor operation instructions in the Atlas Suppressor Manual Section 3, “Operation,” before you start operating the suppressor.
D. See the Atlas Suppressor Manual (Document Number 031770) Section 1.4..3, “Selecting the Correct Suppressor and Mode of Operation,” for recommended columns and currents. The red back-pressure coils (Dionex P/N 45878) are PEEK tubing of 1/16-inch o.d. and 0.005-inch i.d. Make sure that each red back pressure coil yields about 40-50 psi pressure drop at the flow rate of 1.0 mL/min. by completing the test described in Section 1.2, “Back Pressure Coil Test for Dionex Suppressors.”
Figure 1
Figure 2
Cell
READ THIS FIRSTTABLE 1
ATLAS ELECTROLYTIC SUPPRESSOR(AES)
QUICKSTART
Number ExpectedColumn Flow Rate of Red Presure ID PEEKFormat mL/min Coils psi Liquid Line ID 2-mm 0.25 to 0.50 2 20-50 0.005" 3-mm 0.50 to 1.00 2 40-100 0.005" 4-mm 1.00 to 2.00 1 40-100 0.010"