Page 1 Thermo Scientific Dionex Integrion HPIC System Operator’s Manual 22153-97003 Revision 04 August 2016...
Page 2 © 2016 Thermo Fisher Scientific Inc. All rights reserved. Chromeleon and ERS are registered trademarks of Thermo Fisher Scientific Inc. in the United States. Acrobat, Adobe, and Adobe Reader are registered trademarks of Adobe Systems Incorporated in the United States and other countries.
Page 3: Table Of Contents
Notice on Lifting and Handling of Thermo Scientific Instruments ..xvii Notice on the Proper Use of Thermo Scientific Instruments ... . xvii WEEE Compliance ......... . .xviii Conformité...
Page 4 Diluting Samples ..........54 Loading Samples into the Loop or Concentrator ......54 Dionex Integrion Operator’s Manual Thermo Scientific...
Page 5 Annual Maintenance ..........108 Thermo Scientific...
Page 6 Replacing a Dionex CR-TC 600 ....... . . 197 Dionex Integrion Operator’s Manual Thermo Scientific...
Page 7 Appendix B Reordering Information ..........225 Thermo Scientific...
Page 8 Contents Dionex Integrion Operator’s Manual Thermo Scientific...
Page 9: Preface
In addition to this guide, the following related documents are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). • Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002) • Dionex AS-AP Autosampler Operator’s Manual (Document No. 065361) • Dionex AS-DV Autosampler Operator’s Manual (Document No. 065259) •...
Page 10: Safety Information
Note Highlights information of general interest. Tip Highlights helpful information that can make a task easier. Safety Symbols These symbols appear on the Dionex Integrion HPIC System or on labels affixed to the system: Alternating current. Primary protective conductor terminal.
Page 11: Regulatory Compliance
“International Compliance” page The CE mark on the model/data label of the Dionex Integrion HPIC System indicates that the system is in compliance with the following European Union Directives as is evidenced by compliance to the associated standard where appropriate: •...
Page 12: Fcc/Ic Notices
Cet appareil est conforme à la partie 15 des règles de la FCC et d'Industrie Canada RSS normes exemptes de licence. Le fonctionnement de cet appareil est soumis à la deux conditions suivantes: 1. Ce dispositif ne doit pas causer d'interférences nuisibles, et Dionex Integrion Operator’s Manual Thermo Scientific...
Page 13: International Compliance
Wi-Fi module RFID module Dionex Integrion Gainspan GS2011M Skyetek (now Jadak) SM-NV Dionex Integrion RFIC 1219-16-3693 1431-16-2716 India System Wi-Fi module RFID module Dionex Integrion Gainspan GS2011M Jadak SM-NV ETA-824/2016/ERLO ETA-876/2016/ERLO Dionex Integrion RFIC Thermo Scientific Dionex Integrion Operator’s Manual...
Page 14 Dealer’s Licence No. N0375-16 Dealer’s Licence No. N0374-16 Thailand System This telecommunication equipment is in compliance with NTC requirements. System Dionex Integrion REGISTERED No: DA48560/16 DEALER No: ER44279/16 Dionex Integrion RFIC REGISTERED No: DA48560/16 DEALER No: ER442266/16 Dionex Integrion Operator’s Manual Thermo Scientific...
Page 15: Notice On Lifting And Handling Of Thermo Scientific Instruments
Preface Notice on Lifting and Handling of Thermo Scientific Instruments For your safety, and in compliance with international regulations, the physical handling of this Thermo Fisher Scientific instrument requires a team effort to lift and/or move the instrument. This instrument is too heavy and/or bulky for one person alone to handle safely.
Page 16: Weee Konformität
Richtlinie 2002/96/EC. Es ist mit dem folgenden Symbol gekennzeichnet: Thermo Fisher Scientific hat Vereinbarungen mit Verwertungs-/Entsorgungsfirmen in allen EU-Mitgliedsstaaten getroffen, damit dieses Produkt durch diese Firmen wiederverwertet oder entsorgt werden kann. Weitere Informationen finden Sie unter www.thermoscientific.de/rohs. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 17 CAUTION Symbol VORSICHT ATTENTION PRECAUCION AVVERTENZA CAUTION Electric Shock: This instrument uses Elektroschock: In diesem Gerät werden Choc électrique: L’instrument utilise des Descarga eléctrica: Este instrumento Shock da folgorazione. L’apparecchio è high voltages that can cause personal Hochspannungen verwendet, die tensions capables d’infliger des blessures utiliza altas tensiones, capaces de alimentato da corrente ad alta tensione...
Page 18 CAUTION Symbol CAUTION Electric Shock: This instrument uses high voltages that can cause personal injury. Before servicing, shut down the instrument and disconnect the instrument from line power. Keep the top cover on while operating the instrument. Do not remove protective covers from PCBs. Chemical: This instrument might contain hazardous chemicals.
Page 19: Chapter 1 Introduction
Figure Figure 1. Ion analysis process Eluent 4. Detection Suppressor Cell (optional) 3. Separation Separator 1. Eluent delivery column Waste 2. Sample injection Injection valve Guard column (optional) Pump Waste 5. Data analysis Sample Thermo Scientific Dionex Integrion Operator’s Manual...
Page 20: Sample Injection
• As the eluent and sample are pumped through the analytical column, the sample ions are separated. In the Dionex Integrion HPIC System, the mode of separation is called ion exchange chromatography. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites.
Page 21: Deionized Water Requirements For Ic
* Iron/transition metal content not specified for ASTM Type I Water Introduction to the Dionex Integrion The Dionex Integrion HPIC System is an integrated HPIC (high-pressure ion chromatography) system that provides the components and electronics required for performing a wide range of ion analysis applications. The basic system includes an eluent area,...
Page 22: Standard System Configurations
• Eluent area and reservoir • System status LEDs • Pump compartment with analytical pump installed • Column compartment with 6-port injection valve installed ™ ™ • Detector compartment with either a Thermo Scientific Dionex Integrion Conductivity ™ ™ Detector (CD) or Thermo Scientific...
Page 23: Options
The following items can be ordered at any time and installed on-site by Thermo Fisher Scientific field service personnel: • Dionex eluent generator (EG) for generating high purity acid or base eluents online from deionized water • Eluent degas system for continuous, online eluent degassing Thermo Scientific Dionex Integrion Operator’s Manual...
Page 24: Customer-Installable Options
Electrolytic devices include the suppressor, eluent generator cartridge (Thermo Scientific Dionex EGC), continuously-regenerated trap column (Thermo Scientific Dionex CR-TC 600), electrolytic pH modifier (Thermo Scientific Dionex EPM), and electrolytic water polisher. Customer-Installable Options The following options can be ordered any time and installed on-site by either Thermo Fisher Scientific field service personnel or by the customer: •...
Page 25 Introduction Options ™ ™ • The Thermo Scientific Dionex Integrion HPIC Mobile App installed on the optional mobile device can be used for controlling basic instrument functions and for displaying system status information. The mobile app can display a real-time plot of detector output, but it cannot store data or provide data processing functions.
Page 26 Introduction Options Dionex Integrion Operator’s Manual Thermo Scientific...
Page 27: Functional Description
Functional Description This chapter describes the principal components of the Dionex Integrion HPIC System and their functions. Contents • System Overview • Status LEDs • Mobile Device • Chromeleon 7 Chromatography Data System • Electrolytic Device Connections • Consumable Device Tracking •...
Page 28: System Overview
Functional Description System Overview System Overview Figure 3 shows the principal operating components of a Dionex Integrion HPIC System configured for conductivity detection. Figure 3. Example interior components of a Dionex Integrion Eluent area Dionex EGC (optional) Mobile device Additional EG components...
Page 29: Status Leds
For details about the mobile app, see “Dionex Integrion Mobile App Operation” page Figure 4. Example mobile app Home page for a conductivity detection system Thermo Scientific Dionex Integrion Operator’s Manual...
Page 30: Chromeleon 7 Chromatography Data System
Figure 5. Example Chromeleon ePanel Set For instructions on how to connect to the ePanel Set, see “Connecting to Chromeleon” page Dionex Integrion Operator’s Manual Thermo Scientific...
Page 31 Instrument toolbar above the ePanel Set or press the F8 key to open the Chromeleon Command window (see Figure 6). From there, you can access all commands available for the system. Figure 6. Chromeleon Command window Thermo Scientific Dionex Integrion Operator’s Manual...
Page 32: Electrolytic Device Connections
Dionex EGC CR-TC Dionex CR-TC 600 or Dionex EPM AUX 1 Dionex CR-TC 600, electrolytic suppressor, or auxiliary power supply AUX 2 Dionex EGC or auxiliary power supply Requires a Dionex EGC 500 K Dionex Integrion Operator’s Manual Thermo Scientific...
Page 33: Consumable Device Tracking
Last date the device can be installed in the EGCs system before additional validation tests are recommended to ensure proper operation. Lot number Devices that contain Manufacturing lot of the resin used in the resin: guard and device. separator columns, etc. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 34: Installation
Number of sample injections that have concentrator and occurred while the device was installed in the trap columns, system. The count increments when the Dionex EGCs injection valve is switched from Load to Inject during a sequence. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 35 Load to Inject during a sequence and a concentrator column is installed on the valve. Total volume Concentrator Total volume of sample (in mL) injected concentrated columns through the concentrator column in its lifetime. Uses sample volume entered in Chromeleon injection. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 36 Total voltage hours Constant current Total number of hours voltage has been seen suppressors applied to the suppressor during its lifetime. Ion count Dionex EGC Ions remaining in the Dionex EGC, expressed as a percentage. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 37: Eluent Reservoirs
2-liter reservoir location The following reservoirs are available for use with the Dionex Integrion HPIC System: • 2-liter reservoir (P/N 062510) • 4-liter reservoir (P/N 063292) CAUTION Do not use the plastic reservoirs for offline vacuum degassing of eluents. The reservoirs were not designed for this purpose.
Page 38: Pump Compartment Features
The pump is a low-pulsation, serial dual-piston pump with electronic compressibility compensation. Pump flow components are chemically inert, made with high-quality PEEK™ heads and fittings, inert polymer seals, sapphire pistons, and sapphire check valve components. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 39: Static Mixer
9. In this case, the trap column will function as the pulse damper. Table 6 lists the Thermo Scientific high-pressure trap columns available for use with the Dionex Integrion. For details about a column, refer to the column manual. Column manuals are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 40: Pump Seal Wash System
A Seal Wash Kit (P/N 22153-62010) is available that provides the parts for adding a seal wash system to the Dionex Integrion HPIC System. For installation instructions, refer to Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002) provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 41 The Dionex EGC, Dionex CR-TC 600, Dionex EPM, and eluent degasser are installed in the eluent area of the Dionex Integrion HPIC System (see Figure 10).
Page 42: Eluent Generator Cartridge (Dionex Egc)
074535 Methanesulfonic acid Standard pressure For more information, refer to the Dionex EGC manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). You can select the concentration of eluent to be generated from either Chromeleon or from the mobile app Home page. For details, see “Operating the EG”...
Page 43: Continuously Regenerated Trap Column (Dionex Cr-Tc)
K and KHCO eluent. For more information about these products, refer to the Dionex EGC manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 44: Column Compartment Features
For additional temperature specifications, see “Temperature Control Zones” page CAUTION Before servicing the instrument, allow heated components to cool. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 45: High-Pressure Valves
Eluent flows from the pump, through the valve, and to the column, bypassing the sample loop. • In the Inject position, eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 46 Figure 14. 6-port and 10-port high-pressure valve flow schematics A Position B Position A Position B Position 6-port valve 10-port valve Connections from chromatography components to the valve ports depend on the application to be run. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 47: Detector Compartment Features
In addition, the alert LED on the front panel lights. For troubleshooting information, see “Liquid Leaks” page 138. Leaks from the detector compartment, pump compartment, column compartment, and the top front section of the eluent area are all directed to this leak sensor. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 48: Conductivity Detector (Cd)
You can set the compensation factor in Chromeleon or on the mobile app Detector page (see “Detector Page” page 88). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 49: Suppressors, Crd, And Srn
A suppressor is used in conductivity detection applications to reduce the eluent conductivity and enhance the conductivity of the sample ions, thereby increasing detection sensitivity. The ™ CD can operate with a variety of suppressors, including the Thermo Scientific Dionex ERS ™ 500 Electrolytically Regenerated Suppressor and Thermo Scientific Dionex CRS Chemically Regenerated Suppressor.
Page 50 , there is no restriction on the concentration of organic solvents that can be used with ® them (providing the solvent is compatible with PEEK tubing). There is also no restriction on the use of organic solvents when disposable gold electrodes on PTFE substrate and PTFE gaskets are used. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 51: Combination Ph - Ag/Agcl Reference Electrode
The palladium hydrogen electrode becomes a reference electrode with a half reaction of: + e- = ½ H Where the hydrogen is supplied by the following process:   Pd + ½ H Pd-H Pd-H Thermo Scientific Dionex Integrion Operator’s Manual...
Page 52: Temperature Control Zones
Minimum temperatures are also affected by the ambient humidity. If the humidity is high, the minimum temperature achieved for a temperature zone is not as low as that achieved in a low ambient humidity environment. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 53: Rear Panel Features
A kit (P/N 078520) that includes the regulator, mounting bracket, and other items needed must be ordered separately. For installation instructions, refer to Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002) provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 54: Tubing Chase And Waste Lines
Dionex Integrion. IMPORTANT For correct drainage, make sure the drain line is not bent, pinched, or elevated at any point. Do not allow the end of the line to be submerged in waste liquid. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 55: Low-Pressure Valve Connectors
A 1.8 m (6 ft) USB cable (P/N 960777) is included in the Dionex Integrion Ship Kit (RFIC, P/N 22153-62003; non-RFIC, P/N 22153-62002). For connection instructions, refer to Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002), provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 56: Low-Pressure Valve Options
To control the valves, use one of the following methods: • Select commands on the Pump_ECD ePanel in Chromeleon. • Select commands on the mobile app Valves page. • Add commands to a Chromeleon instrument method. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 57: System Flow Schematics
• Conductivity detection using suppression in recycle mode with Reagent-Free IC eluent generation (RFIC-EG); cation system (see Figure • Conductivity detection using suppression in recycle mode with RFIC-EG; anion system (see Figure • Electrochemical detection with RFIC-EG (see Figure Thermo Scientific Dionex Integrion Operator’s Manual...
Page 58: Column Compartment
VALVE PRIMARY HEAD PRIME SHUTOFF WASTE VALVE SECONDARY HEAD PRE-BENT INJECTION MIXER VALVE DETECTOR COMPARTMENT CONDUCTIVITY DETECTOR ELUENT TO WASTE REGEN FROM AUTOSAMPLER BACK- PRESSURE COIL SUPPRESSOR REGEN ELUENT FROM COLUMN OUT TO WASTE Dionex Integrion Operator’s Manual Thermo Scientific...
Page 59 VALVE PRIMARY HEAD PRIME SHUTOFF WASTE VALVE SECONDARY HEAD MIXER PRE-BENT INJECTION VALVE DETECTOR COMPARTMENT CONDUCTIVITY DETECTOR ELUENT TO WASTE FROM AUTOSAMPLER REGEN BACK- PRESSURE COIL SUPPRESSOR REGEN ELUENT TO WASTE FROM COLUMN OUT Thermo Scientific Dionex Integrion Operator’s Manual...
Page 60 PRIME SHUTOFF WASTE VALVE SECONDARY HEAD MIXER PRE-BENT INJECTION VALVE DETECTOR COMPARTMENT CONDUCTIVITY DETECTOR ELUENT TO WASTE REGEN FROM AUTOSAMPLER ELUENT BACK- REGEN PRESSURE COIL REGEN ELUENT REGEN ELUENT TO WASTE FROM COLUMN OUT Dionex Integrion Operator’s Manual Thermo Scientific...
Page 61 PUMP COMPARTMENT DEGAS ELUENT PRE-HEATER PRIMING VALVE PRIMARY HEAD PRIME SHUTOFF WASTE VALVE SECONDARY HEAD MIXER PRE-BENT INJECTION VALVE DETECTOR COMPARTMENT ELECTROCHEMICAL DETECTOR TO WASTE FROM AUTOSAMPLER ELUENT ELUENT TO WASTE FROM COLUMN OUT Thermo Scientific Dionex Integrion Operator’s Manual...
Page 62 Functional Description System Flow Schematics Dionex Integrion Operator’s Manual Thermo Scientific...
Page 63: Operation
Integrion HPIC System has already been completed (including configuring the Dionex Integrion HPIC System in a Chromeleon instrument). If this is not the case, refer to Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002) for instructions before beginning operation.
Page 64: Starting Up The System (Overview)
6. Install the reservoir cap, making sure the end of the line extends to the bottom of the reservoir, and that the filter is submerged in liquid. This prevents air from being drawn through the eluent lines. Hand-tighten the cap. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 65 The gas regulator accessory bracket and other items needed for pressurizing the eluent reservoir must be ordered separately (P/N 078520). For installation instructions, refer to Dionex Integrion HPIC System Installation Instructions (Document No. 22153-97002) provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 66 VORSICHT Setzen Sie den Eluentbehälter auf keinen Fall einem Druck über 0,07 MPa aus. 6. If the liquid line from the pump is connected, you may open the gas shutoff valve on the reservoir cap. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 67: Setting Up The Seal Wash System
To display the ePanel Set Click the Instruments Category Bar. Select the name of the instrument in which the Dionex Integrion is configured. Chromeleon connects to the instrument and displays the ePanel Set. See the example in Figure Thermo Scientific Dionex Integrion Operator’s Manual...
Page 68: Priming The Pump
Figure 26) by turning the knob one-half turn counterclockwise. Note If the priming valve is opened too much, air is drawn through the valve and air bubbles can be seen exiting the waste line. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 69 7. Enter the flow rate required for your application and turn on the pump flow. 8. After starting the pump, wait at least 5 minutes (longer for flow rates below 1.0 mL/min) before beginning an analysis. This allows the pump to stabilize the flow rate. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 70: Equilibrating The System
5. Verify that the detector baseline is at the expected reading for your application and is stable. Refer to the column manual for the appropriate background for your application. The column manuals are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 71: Preparing Samples
In general, samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant change in anion concentration. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 72: Pretreating Samples
Refer to the installation and troubleshooting guide for the OnGuard cartridge for instructions. The guide is provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Diluting Samples Because the concentrations of ionic species in different samples can vary widely from sample to sample, no single dilution factor can be recommended for all samples of one type.
Page 73 2. Prepare and fill the sample vials or well plates and place them in the autosampler tray or carousel. For detailed instructions, refer to the autosampler manual, provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). 3. Create a sequence in Chromeleon that specifies the vials or wells from which to take sample injections and the order in which the injections should be run.
Page 74: Performing Sample Analyses
• The Sequence Wizard provides a series of dialog boxes that guide you through the sequence creation process. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 75: System Shutdown
The columns, suppressors, and other consumable items used with the Dionex Integrion have various short- and long-term storage requirements. Refer to the manuals for the individual products for instructions. These manuals are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 76: Operating The Eg
Dionex EGC 500 K For 4 mm operation: Up to 15 mM K at 1.0 mL/min; up to 7.5 mM K at 2.0 mL/min For 2 mm operation: Up to 15 mM K at 0.25 mL/min Dionex Integrion Operator’s Manual Thermo Scientific...
Page 77: Entering The Eluent Concentration
For 2 mm operation: Up to 100 mM MSA at 0.25 mL/min For the eluent concentration required for your application, refer to the column manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Entering the Eluent Concentration The eluent concentration can either be programmed into a Chromeleon instrument method (for automated operation) or entered on the Chromeleon ePanel Set or mobile app (for direct control of the Dionex EGC).
Page 78: Operating The Ed
• Replace the PdH reference electrode if its sensing surface is damaged or if the electrode no longer seals properly. Replace the PdH electrode if performance has degraded; for example, you observe lower response, higher background, or spikes. The PdH reference electrode typically lasts several years, depending on use. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 79 Ag/AgCl reference potential. 4. If the pH value shifts by 0.5 pH unit from the value first observed, check the pH-Ag/AgCl reference electrode. See “To determine a reference potential shift” page 148. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 80: Electrochemical Detection Modes
Electrochemical Detection Modes The Dionex Integrion Electrochemical Detector can perform the following electrochemical detection modes: • DC amperometry (see page • Integrated amperometry, including pulsed amperometric detection (PAD) and integrated pulsed amperometric detection (IPAD) (see page Dionex Integrion Operator’s Manual Thermo Scientific...
Page 81: Dc Amperometric Detection
Current is measured by integration during a portion of the repeating potential vs. time waveform. For more information about waveforms, see page Thermo Scientific Dionex Integrion Operator’s Manual...
Page 82 (see Figure 33). Figure 33. Example integrated pulsed amperometry waveform +0.60 +0.35 Potential (Volts) -0.10 Integration -0.60 E1, E2. Detection Potentials Time (Seconds) E3. Positive Cleaning Potential E1, E2 E4. Negative Cleaning Potential Dionex Integrion Operator’s Manual Thermo Scientific...
Page 83: Waveforms
(alcohols, amino acids, carbohydrates, etc.) can be included in a Chromeleon instrument method. The waveforms can also be selected on the mobile app “Electrolytics Page” page 92. In the Chromeleon Waveform Editor, you can modify a pre-programmed waveform or define a new waveform. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 84: Collecting And Storing Amperometry Data
18 mM NaOH Flow Rate: 1.5 mL/min Detection: Pulsed Amperometry Electrode: Gold Waveform: Quadruple Potential Peaks: 1. L-Fucose 2. D-Galactosamine 3. D-Glucosamine 4. D-Galactose 5. D-Glucose Response 6. D-Mannose (nC) Minutes Retention Time (Minutes) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 85: Using Rear Panel Inputs And Outputs
TTL output #2 (332  pull up to +5 V, 100 mA sink) Digital ground TTL output #1 (332  pull up to +5 V, 100 mA sink) Note: Relays are capable of switching 2 A at 24 VDC. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 86 2. For each I/O function to be used, connect an active wire (red) and a ground wire (black) to the connector plug at the pin locations for the selected I/O function. See Table 11 the label on the rear panel for the connector pin assignments for each I/O function. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 87: Assigning Ttl Input Functions
TTL/Relay page. When connected to a controlling device, the device can send a signal to the TTL input to trigger the assigned functions.  To select TTL input functions from Chromeleon 1. Open the Chromeleon Instrument Configuration Manager. 2. Double-click the Dionex Integrion HPIC System icon under the instrument. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 88 6. If the device connected to the TTL input does not send a normal edge signal, select the control type compatible with the device. To determine the correct type, refer to the Dionex Integrion Operator’s Manual Thermo Scientific...
Page 89 The inverted edge mode works identically to the normal edge TTL Inverted Edge mode except that the positive and negative edges are reversed Action on in function. +5 V +0 V Action off or no effect Thermo Scientific Dionex Integrion Operator’s Manual...
Page 90: Controlling Relay And Ttl Outputs
To control a relay or TTL output from Chromeleon 1. On the Chromeleon ePanel Set, click the Pump_ECD tab. 2. Click the Relays/TTL button (see Figure 39). Under Output Relays and TTLs, select the TTL output and relay output settings. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 91: Selecting Analog Output Settings
Several settings are available that allow you to configure the analog output signal for your detector and connected device (see Table 12). You can select the preferred settings on the Chromeleon ePanel (see Figure 40) or the mobile app Analog page (see “Analog Page” page 98). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 92 10% of the full-scale Use this setting to send a positive pulse to command only) analog output the analog output as an event marker. A mark is typically used to indicate a sample injection. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 93 To select analog output settings from the mobile app 1. On the mobile app quick access toolbar, tap the Accessories icon and then select ANALOG on the menu. 2. Select the analog output parameter settings. For details, see “Analog Page” page Thermo Scientific Dionex Integrion Operator’s Manual...
Page 94 Operation Using Rear Panel Inputs and Outputs Dionex Integrion Operator’s Manual Thermo Scientific...
Page 95: Dionex Integrion Mobile App Operation
• Valves Page • Detector Page • Electrolytics Page • Temperature Page • Plot Page • Analog Page • TTL/Relay Page • TTL Input Page • Consumables Page • Calibration Pages • Information Page Thermo Scientific Dionex Integrion Operator’s Manual...
Page 96: Overview Of Mobile App Operation
Overview of Mobile App Operation Overview of Mobile App Operation The mobile app provides direct control of most Dionex Integrion HPIC System operating functions. When you select an operating command or parameter from the mobile app, the command or parameter is executed immediately.
Page 97: Quick Access Toolbar
Tap the icon to see the error. You can view error messages either one at a time (see Figure 44) or in a list view (see Figure 45). For troubleshooting information about an error message, see “Troubleshooting Error Messages” page 109. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 98: Using The Mobile App With Chromeleon
However, if you attempt to change an operational setting from the mobile app, a message warns you that you are about to interrupt a running sequence. You can choose to stop the running sequence or wait until the sequence is finished. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 99: Home Page Details
Tap the AUTOZERO button to set the reading to zero. Tap the button to control the cell heater, enter a rise time, or enter a temperature compensation factor (see “Conductivity Detector (CD)” page 88). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 100 Tap the AUTOZERO button to set the reading to zero. Tap the button to monitor the total current reading or change the detector mode (see “Electrochemical Detector (ED)” page 90). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 101 Displays a thumbnail view of the current plot. Tap the button to view the plot on a full page and select additional parameters (see “Plot Page” page 96). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 102: Pump Page
Toggles the priming function off and on. flow rate button Indicates/sets the priming flow rate. Tap the down arrow to select a different flow rate. For detailed priming instructions, see “Priming the Pump” page Dionex Integrion Operator’s Manual Thermo Scientific...
Page 103 (always on). VACUUM OK (or Indicates the status of the vacuum. If the vacuum is not okay, see VACUUM NOT OK) the troubleshooting information in “Degas Vacuum Pump Low Vacuum” page 145. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 104 Accessory Controls Figure 47. Accessory controls Seal Wash Pump Control Description INTERVAL (ON) Determines whether the pump will run in intervals or is off. button PRIME button Toggles seal wash pump priming off and on. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 105: Valves Page
Indicates the current position of each installed valve. To change the position, tap the button. Time value (min) • High-pressure valves: Indicates the elapsed time from the last injection. • Low-pressure valves: Indicates the elapsed time from the last valve position change. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 106: Detector Page
Indicates the total conductivity (without a background offset). CONDUCTIVITY CELL Toggles the cell heater on and off. TEMPERATURE STATUS button CELL Indicates/sets the cell heater setpoint. Tap the value to change the TEMPERATURE setting. button Dionex Integrion Operator’s Manual Thermo Scientific...
Page 107 For example, for a peak width of 5 seconds, calculate the rise time as: (5 sec) 25% = 1.25 sec. Because 1.25 sec is not one of the available settings for rise time, select the next fastest rise time, 1 sec. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 108: Electrochemical Detector (Ed)
Dionex Integrion Mobile App Operation Detector Page Electrochemical Detector (ED) Figure 50. ED detector page: Integrated amperometry mode, AgCl reference electrode Figure 51. ED detector page: Integrated amperometry mode, PdH reference electrode Dionex Integrion Operator’s Manual Thermo Scientific...
Page 109: Cell Control
(highlighted in blue). Tap a mode to select it. Two reference electrode types are available for the ED: • Combination pH-Ag/AgCl reference electrode (mode = AgCl or pH) • Palladium hydrogen (PdH) reference electrode (mode = PdH) Thermo Scientific Dionex Integrion Operator’s Manual...
Page 110: Electrolytics Page
The page shows only the electrolytic devices installed in the system. The total number of electrolytic devices that can be installed in a system is determined by the installed power supply option. Power supply options are described on page Figure 53. Electrolytics page example (1-channel option) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 111 Dionex Integrion Mobile App Operation Electrolytics Page Figure 54. Electrolytics page example (3-channel option) Figure 55. Electrolytics page example (5-channel option) Thermo Scientific Dionex Integrion Operator’s Manual...
Page 112 Indicates/sets the eluent concentration setpoint. To change the setpoint, tap the value. To determine the eluent concentration required for your application, refer to the column manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). LIFE (%) Displays the percentage of the remaining ion capacity in the Dionex EGC.
Page 113: Temperature Page
The controls on the page are the same for each device (COMPARTMENT TEMPERATURE, COLUMN HEATER, CD CELL HEATER). Only the devices installed in the system are displayed on the page. Figure 56. Temperature page Thermo Scientific Dionex Integrion Operator’s Manual...
Page 114: Plot Page
• Data acquisition stops for the last signal selected to be plotted. When one of these events occurs, the elapsed time counter, time axis, and data buffer are all reset to zero and the plot restarts. Figure 57. Plot page Dionex Integrion Operator’s Manual Thermo Scientific...
Page 115 If the tops of peaks are cut off, select a higher range. If peaks are short, select a lower range. To have the scaling of the signal plot automatically adjust to the height of the signal, select AUTO. The range for the pressure signal is always Auto. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 116: Analog Page
Two analog output connectors are provided on the Dionex Integrion rear panel. Each analog output supplies a voltage signal proportional to the current measured by a detector cell. The outputs can be connected to an analog-to-digital (A/D) converter, such as an integrator or other recording device. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 117 (positive) or INVERTED (negative). Tap the button to changed the polarity. In applications in which the analyte output is lower than the background signal, the polarity must be inverted to display peaks instead of dips on the chromatogram. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 118: Ttl/Relay Page
For TTL and relay connection instructions, see “Connecting the I/O Connectors” page  To open the TTL/Relay page On the mobile app quick access toolbar, tap the Accessories icon and then tap TTL/RELAY on the menu. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 119: Ttl Input Page
TTL Input Page Use the TTL Input page to assign functions to the TTL inputs and select input control types.  To open the TTL Input page On the TTL/Relay page, tap the TTL INPUT button. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 120: Consumables Page
EDGE, INVERTED EDGE, NORMAL PULSE, or INVERTED PULSE) to accommodate different controlling devices. The default control type, normal edge, is compatible with the output signals provided by Thermo Scientific Dionex modules. If the controlling device connected to the input does not send a normal edge signal, select the appropriate control type.
Page 121 To enable use of a detected RFID device in the system 1. If a detected RFID device is installed in the system, select its check box. 2. The Rescan button changes to Approve. Tap the button to enable use of the device. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 122: Calibration Pages
“To calibrate the pH-Ag/AgCl reference electrode” page 213.  To open the Calibration page On the mobile app quick access toolbar, tap the Service icon and then tap CALIBRATION on the menu. Figure 63. Calibration page: conductivity cell Dionex Integrion Operator’s Manual Thermo Scientific...
Page 123: Information Page
 To open the Information page On the mobile app quick access toolbar, tap the Service icon and then tap INFORMATION on the menu. Figure 65. Information page Thermo Scientific Dionex Integrion Operator’s Manual...
Page 124 Dionex Integrion Mobile App Operation Information Page Dionex Integrion Operator’s Manual Thermo Scientific...
Page 125: Chapter 5 Maintenance
Note It is especially important to regularly replace end-line filters when using aqueous eluents, which may contaminate the filter with bacteria or algae. The bacterial buildup may not be visible. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 126: Periodic Maintenance
5. Dry the reservoir with clean, particulate-free air. Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually, as well as before scheduled Performance Qualification tests. A Dionex Integrion HPIC System Preventive Maintenance Kit (P/N 22153-62041) is available for this purpose. Dionex Integrion Operator’s Manual...
Page 127: Troubleshooting
This chapter is a guide to troubleshooting issues that may arise during operation of the Dionex Integrion HPIC System. If you are unable to resolve a problem by following the instructions here, contact Technical Support for Dionex products. In the U.S. and Canada, call 1-800-532-4752.
Page 128 Abort page 115 Camshaft index too late Abort page 115 Camshaft sensor always alight Abort page 116 Camshaft sensor missing or dark Abort page 116 CD cell memory reset to defaults Warning page 116 Dionex Integrion Operator’s Manual Thermo Scientific...
Page 129 123 ED cell reference electrode disconnected Warning page 123 ED cell working electrode disconnected Warning page 124 ED pH offset calibration failed Warning page 124 ED pH slope calibration failed Warning page 124 Thermo Scientific Dionex Integrion Operator’s Manual...
Page 130 131 Motor position error. The motor is overloaded. Abort page 131 No RFID labels found Warning page 131 Pressure fallen below lower limit Abort page 132 Pump is unlinked from Integrion Abort page 132 Dionex Integrion Operator’s Manual Thermo Scientific...
Page 131 This error occurs when there is a diagnostic failure.  To troubleshoot Contact Technical Support for Dionex products for assistance. The control electronics for the electrolytic device may have malfunctioned. Note The Dionex Integrion electronics components cannot be serviced by the user. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 132 Aux_PowerSupply_2 over current This error occurs when an electrolytic device is not properly connected to the auxiliary power supply.  To troubleshoot Verify that the electrical cable from the electrolytic device is connected correctly. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 133 This error occurs when there is an internal error in the pump drive mechanism.  To troubleshoot 1. Turn off the pump power for 30 seconds and then turn it on again. 2. If the error message appears again, contact Technical Support for Dionex products for assistance. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 134 5 °C less than the CD cell temperature setting. 2. Check the suppressor current setting. Running the suppressor at a higher current than is recommended for the application can cause the CD cell to heat up. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 135: Cd Cell Temperature Is Lower Than Expected
This error occurs when the temperature of the column heater exceeds the maximum allowed. This error may occur if the system is operating in an environment in which the temperature is greater than 40 °C.  To troubleshoot For environmental specifications, see Appendix A, “Specifications.” Thermo Scientific Dionex Integrion Operator’s Manual...
Page 136: Column Heater Memory Reset To Defaults
Contact Technical Support for Dionex products for assistance. Column temperature sensor error This error indicates that the temperature sensor in the column compartment is not working properly.  To troubleshoot Contact Technical Support for Dionex products for assistance. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 137: Cr-Tc/Epm Cartridge Disconnected
CR-TC 600 is interrupted.  To troubleshoot 1. Verify that the Dionex CR-TC 600 is securely plugged in (see Figure 66). 2. If the pump stopped unexpectedly, follow the troubleshooting steps in “Pump Stops” page 145. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 138: Cr-Tc Short Circuit
Dionex CR-TC 600) are on. The Dionex CR-TC 600 current is automatically turned off to prevent damage to the Dionex CR-TC 600.  To troubleshoot If the pump stops unexpectedly, follow the troubleshooting steps in “Pump Stops” page 145. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 139: Detector Compartment Door Opened
To troubleshoot 1. Repeat the calibration procedure. Follow the instructions provided in the Dionex Integrion Temperature Calibration Kit (P/N 22153-62043). 2. If the error message appears again, contact Technical Support for Dionex products for assistance. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 140: Detector Compartment Temperature Is Lower Than Expected
5. Restart the flow and select the DC amperometry mode. Apply cell potential in steps increasing toward the detection potential (the potential of the integration period in integrated amperometric detection). If the current becomes excessive again, try a new working electrode or another cell, if available. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 141: Ed Cell Memory Reset To Defaults
(see Figure 67). Figure 67. Detector compartment features ( ED configuration) Reference electrode electrical cable ED cell electrical cable Reference electrode (pH–Ag/AgCl version shown) ED cell Thermo Scientific Dionex Integrion Operator’s Manual...
Page 142: Ed Cell Working Electrode Disconnected
4. If the error recurs after repeating the calibration at least two times, replace the Ag/AgCl reference electrode (see page 211 for instructions). Note The following error is applicable to EG, EG2 and EG3 consumable inventory cable access: Dionex Integrion Operator’s Manual Thermo Scientific...
Page 143 Wait for a few seconds, and then plug in the cable again. 2. If the error message appears again, replace the cartridge. 3. If the error message appears again, contact Technical Support for Dionex products. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 144 Dionex EGC.  To troubleshoot 1. Verify that the Dionex EGC cable is securely plugged in (see Figure 66). 2. If the error message appears again, contact Technical Support for Dionex products for assistance. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 145 1. To determine why liquid flow stopped, see “Pump Stops” page 145. 2. If the error message appears again, contact Technical Support for Dionex products for assistance. The Dionex EGC control electronics may have malfunctioned. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 146 This error occurs when the high-pressure valve receives a command before it has completed the action required by a previous command.  To troubleshoot Wait until the previous action has been completed, and then retry. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 147 Invalid flow value This error occurs when you attempt to select a flow rate that is outside the valid flow rate range.  To troubleshoot Enter a valid flow rate (see “Specifications” page 221). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 148: Leak Sensor Wet
4. If the problem persists, contact Technical Support for Dionex products for assistance. Load/Inject valve busy This error occurs if the injection valve has not yet completed the required action.  To troubleshoot Wait until the previous action has been completed, and then retry. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 149 (If an RFID consumable is not currently being tracked, the button label is Track and Get Details). Refer to the Chromeleon Help for details. • For mobile app operation: Tap the Rescan button on the Consumables page. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 150 1. Check the orientation of all the RFID labels on the installed consumable products. Labels should be free in the air (not wrapped around a column or caught behind something). 2. If the error message appears again, contact Technical Support for Dionex products for assistance. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 151 2. Inspect the outlet check valve for blockage. Replace the check valve cartridge if needed (see “Replacing Pump Check Valves” page 183). Suppressor not installed This error occurs when the suppressor is on, but no suppressor is detected.  To troubleshoot Verify that the suppressor is installed correctly. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 152: Suppressor Over Current
 To troubleshoot 1. Follow the instructions in the suppressor manual to regenerate the suppressor. Suppressor manuals are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). 2. Follow the instructions in the suppressor manual to clean the suppressor.
Page 153 2. To determine the source of the high backpressure, isolate segments of the flow path: a. Remove the pump outlet tubing at the injection valve. b. Turn on the pump. c. On the Chromeleon ePanel Set, set the flow rate to 1.0 mL/min. Record the backpressure. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 154 If the column is the source of the high backpressure, clean the column. (Refer to the column manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891) for instructions.) If this does not eliminate the problem, replace the column.
Page 155: Troubleshooting System Component Symptoms
If the column is the source of the high backpressure, clean the column. (Refer to the column manual provided on the Thermo Scientific Reference Library DVD (P/N 60-053891) for instructions.) If this does not eliminate the problem, replace the column.
Page 156: Troubleshooting
Verify that the system is configured in Chromeleon and is Chromeleon assigned to an instrument. For Chromeleon configuration instructions, refer to Dionex Integrion HPIC System Installation Instructions or to the Chromeleon Help. Microsoft Windows power When the power management option is enabled, the PC management option automatically turns off power to USB devices that are idle.
Page 157 2. If the knob leaks when closed, replace the seal. 3. If the leak still occurs, either the pump head or the knob is damaged and should be replaced. Contact Technical Support for Dionex products for assistance. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 158: Low Or Decreasing System Backpressure
To determine the source of the leak, see “Liquid Leaks” flow path page 138. Eluent supply depleted Check the eluent reservoir and refill it if needed. Prime the pump before resuming operation (see “Priming the Pump” page 50). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 159 Dionex EGC (see “Replacing a Dionex EGC” page 193). Note The leak sensor cannot immediately detect leakage from the membrane barrier, as these leaks exit through the Dionex EGC vent line. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 160: High Or Increasing System Backpressure
4. One at a time, reconnect each component of the flow path. Refer to the flow schematic on the inside door of your system or to the following figures: – For conductivity detection, see Figure 19 Figure 20 (if an EG is installed). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 161 (see “Rebuilding a High-Pressure Valve” page 199). Dionex EGC III Replace the outlet frit as instructed in the Dionex EGC manual. The manual is provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 162: Unstable System Backpressure
If the injection valve is the suspected source of the unstable backpressure, the injection valve rotor seal or stator may need to be replaced (see “Rebuilding a High-Pressure Valve” page 199). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 163: Pump Does Not Start
142. Degas Vacuum Pump Low Vacuum Possible cause Solution Leak in the vacuum degas Check all tubing connections for leakage; tighten loose fitting module connections (see “Fitting and Tube Connection Guidelines” page 180). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 164: Degas Vacuum Pump Does Not Run
Degas Vacuum Pump Does Not Run Possible cause Solution Degas option disabled 1. Open the Chromeleon Instrument Configuration Manager, right-click the Dionex Integrion HPIC System device in the instrument, and select Properties 2. Click the tab and verify that the...
Page 165: Ed Cell Ph Readouts Incorrect
Chromeleon, the Chromeleon instrument method, or the mobile app Home page. Disconnected reference electrode Verify that the reference electrode cable is securely connected. Uncalibrated pH-Ag/AgCl Calibrate the electrode (see page 213). reference electrode Thermo Scientific Dionex Integrion Operator’s Manual...
Page 166 To determine a reference potential shift 1. For each pH-Ag/AgCl reference electrode (the unexposed electrode and the electrode being tested), use a straightened paper clip or short piece of wire of a suitable diameter to Dionex Integrion Operator’s Manual Thermo Scientific...
Page 167: Troubleshooting Chromatogram Symptoms
Varying Peak Retention Times page 166 Peak Results: Unknown peak Unknown Peaks page 168 Peak Results: Missing peak Missing Peaks page 169 Baseline Noisy Baseline page 171 Drifting Baseline page 173 High Background page 174 Thermo Scientific Dionex Integrion Operator’s Manual...
Page 168: Tailing Peaks
• The eluent being used is supported. • The correct eluent concentrate was used when preparing the eluent. • The correct EGC type is installed and the correct EGC type is selected. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 169 ) is the backpressure at the eluent out port. If the pressure is above 0.7MPa (100 psi), find and eliminate the cause of the excessive backpressure (see “High or Increasing System Backpressure” page 142). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 170 2. If you are using a conventional working electrode, polish the electrode (see “Polishing a Conventional Working Electrode” page 209). If you are using a disposable electrode, replace it; see Appendix B, “Reordering Information.” Dionex Integrion Operator’s Manual Thermo Scientific...
Page 171: Fronting Peaks
After removing a column from the system, always install column plugs. When shutting down a system for more than one week, follow the storage recommendation procedures provided in the column manual. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 172 ) is the backpressure at the eluent out port. If the pressure is above 0.4 MPa (60 psi), find and eliminate the cause of the excessive backpressure (see “High or Increasing System Backpressure” page 142). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 173 2. If cleaning the suppressor does not eliminate the problem, the suppressor may need to be replaced. 3. To prevent contamination, install a trap column or use a sample preparation procedure before injection. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 174: Low Efficiency (Peak Broadening)
2. If cleaning the column does not eliminate the problem, the column may need to be replaced. 3. To prevent contamination, install a trap column or use a sample preparation procedure before injection. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 175 High sample concentration Although peak fronting is the most common result of sample or high sample volume overloading, peak broadening can also occur. Dilute the sample (see “Diluting Samples” page 54) or inject a smaller volume. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 176: Loss Of Resolution
6. Regenerate the eluent trap column, or install a new trap column between the pump and the injection valve. 7. For an EG: Check the Dionex EGC settings and verify that the correct cartridge type is selected. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 177 A degradation of peak shape can cause loss of efficiency resolution even if the retention times of the analytes are not affected (see “Tailing Peaks” page 150, “Fronting Peaks” page 153, or “Low Efficiency (Peak Broadening)” page 156). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 178 • Alcohols in the eluent or sample: Some cation separator columns, such as the Dionex IonPac CS12A and CS16, are incompatible with alcohols. Newer columns, such as the Dionex IonPac CS17, are compatible with alcohols. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 179: Split Peak Or Dip
2. Dry with clean, particulate-free air. 3. If the reservoir still appears dirty, or if there is a slimy film on the interior, follow the cleaning instructions on page 108. 4. Replace the end-line filter (P/N 045987). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 180 4. Use a hydroxide eluent: Hydroxide eluents typically do not have a carbonate dip, but instead have a carbonate peak. To eliminate or reduce the carbonate peak from a hydroxide system, install a Dionex CRD 200. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 181 After removing a column from the system, always install column plugs. When shutting down a system for more than one week, follow the storage recommendation procedures provided in the column manual. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 182: Low Detector Output
Recalibrate the pH-Ag/AgCl reference electrode (see page 213). If the problem persists, replace the pH-Ag/AgCl reference electrode (see page 211). Analog output range set Select a more sensitive analog output range. too high Dionex Integrion Operator’s Manual Thermo Scientific...
Page 183: Non-Reproducible Peak Area
For troubleshooting, see the manual for your autosampler. Consider running a performance qualification. Contact Technical Support for Dionex products for assistance. Unstable conductivity cell Verify that the cell temperature control is turned on in temperature the instrument method. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 184: Varying Peak Retention Times
2. Verify that the pump flow rate is correct. 3. Check for other leaks. Temperature fluctuations Check for temperature fluctuations in the ambient temperature and the column and detector compartments. Make sure air conditioning vents do not blow directly onto the instrument. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 185 4. Consider using the Virtual Column Separation Simulator to help better determine the appropriate eluent. To open the simulator, click the command on the Tools menu in the Chromeleon Console. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 186: Unknown Peaks
“Deionized Water Requirements for IC” page 2. Use an alternate water source. 3. Perform preventive maintenance on the current water source. 4. Manually prepare eluent. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 187: Missing Peaks
2. If cleaning the suppressor does not eliminate the problem, the suppressor may need to be replaced. 3. To prevent contamination, install a trap column or use a sample preparation procedure before injection. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 188 Verify that the cell voltage is turned on in the Chromeleon instrument method. If you are operating from the mobile app, turn on the voltage on the Home page. Autosampler leaking For troubleshooting, see the manual for your autosampler. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 189: Noisy Baseline
2. If needed, correct the current or temperature settings and find and eliminate the cause of excessive backpressure (see “High or Increasing System Backpressure” page 142). 3. Consider cleaning the suppressor or replacing the suppressor. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 190 Regenerate the pH-Ag/AgCl reference electrode frit by soaking pH-Ag/AgCl reference the electrode in a solution of 1 M KCl plus 1 M HCl. electrode diaphragm If this does not eliminate the spiking, replace the electrode (causing frequent, random (P/N 061879). spikes) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 191: Drifting Baseline
2. If the conductivity is too high, use an alternate water source or perform preventive maintenance on the current water source. Column is contaminated 1. Clean the column. 2. Replace the inlet bed support. 3. Replace the column. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 192: High Background
Chromeleon instrument method. (CD system) Background Verify that the suppressor is turned on and the current is set to not suppressed by the correct value. Refer to the suppressor manual for additional suppressor troubleshooting guidance. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 193 (see “Replacing a Disposable Working Electrode Gasket” page 206 “Replacing a Conventional Working Electrode Gasket” page 207). 4. Turn the yoke knob (see Figure 95) a full 360 degrees to completely engage the knob. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 194 Troubleshooting Troubleshooting Chromatogram Symptoms Dionex Integrion Operator’s Manual Thermo Scientific...
Page 195: Chapter 7 Service
Service This chapter describes Dionex Integrion HPIC System service and repair procedures that users may perform. Procedures not included here, including electronics-related repair procedures, must be performed by Thermo Fisher Scientific personnel. For assistance, contact Technical Support for Dionex products. In the U.S. and Canada, call 1-800-532-4752.
Page 196: Replacing Tubing And Fittings
1.02 mm (0.040 in) ID tan 054410 • Shutoff valve outlet to primary pump PEEK tubing (4.81 in inlet check valve length) • (RFIC-EG systems) Degas to shutoff valve Dionex Integrion Operator’s Manual Thermo Scientific...
Page 197 1/16 in flangeless fitting nut 052230 1/8 in ferrule 048949 • (CD systems) Suppressor regen ports 1/8 in flangeless fitting nut 057934 • Cell/regen out to waste line (short) 1/4-28 coupler 039056 Waste line Thermo Scientific Dionex Integrion Operator’s Manual...
Page 198: Fitting And Tube Connection Guidelines
2. Insert the tubing into the port until it stops. 3. While maintaining pressure on the tubing to keep it in place in the port, tighten the fitting bolt fingertight and then tighten the fitting further by following the instructions below. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 199: Installing And Tightening Ic Peek Viper Fittings
• For subsequent installations: Use your fingers to tighten the bolt one-sixteenth of a turn from the “0” mark (22° or 4 minutes past 12 on a clock face) (see Figure 81 page 182, View B). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 200: Cutting Tubing
If necessary, order a tubing cutter (P/N 049584) from Thermo Fisher Scientific. Note Do not cut tubing on which IC PEEK Viper fittings are installed. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 201: Servicing Pump Components
Note Never disassemble the pump head with bare hands. Even minute particles of dust, dirt, etc., on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 202 Note For correct pump operation, the check valve cartridges must be installed in their respective housings in the correct orientation. Liquid enters through the check valve in the large single hole and exits through the small double holes. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 203: Replacing Pump Seals
• ASTM Type I (18 megohm-cm) filtered and deionized water that meets the specifications listed in “Deionized Water Requirements for IC” page • Methanol (optional) • 0.2 micron filtered, Class 10, isopropyl alcohol (IPA) • Lint-free paper towels (KIMWIPES or equivalent) • Large flat-blade screwdriver Thermo Scientific Dionex Integrion Operator’s Manual...
Page 204 Main seal (P/N 075768) Seal retainer (P/N 062092) Primary pump head (P/N 075047) Piston (P/N 079857) Inlet check valve assembly Backup ring (P/N 045722) (P/N 074370) (includes valve body O-ring and cartridge) (P/N 040695) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 205 3. Inspect the piston for signs of damage. If the piston is scratched or scored, replace it (see page 190). IMPORTANT Even minute scratches or particles of dust, dirt, etc. on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 206 IMPORTANT Do not use a sharp tool (such as tweezers) to remove the seal wash seal. This may scratch the seal and the inside of the pump housing; scratches will prevent a proper seal and cause leakage. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 207 6. Wet the inside of the pump head cavity where the main seal will be installed with 0.2 micron filtered, Class 10, IPA or ASTM Type I (18 megohm-cm) filtered and deionized water. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 208: Replacing A Pump Piston
1. Turn off the pump flow. 2. Begin monitoring the Pressure reading on the pump ePanel in Chromeleon. When the system pressure reaches zero: • Disconnect the pump from the software by clicking Connected on the ePanel. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 209 4. Reconnect all tubing connections to the pump head. Tighten connections fingertight, and then tighten an additional one-quarter turn only. 5. Close the compartment door. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 210: Replacing The Seal On The Pump Priming Valve Knob
Figure 87. Priming valve knob on secondary pump head Priming valve knob 6. Pull the old seal off the end of the priming valve knob. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 211: Servicing Eluent Generator Components
MISE EN GARDE La cartouche d'EGC contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de . Porter des lunettes et des gants protectives en manipulant la cartouche. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 212 Eluent In ELUENT OUT ELUENT IN Outlet Inlet Vent to To inject valve port P waste To waste/gas separator REGEN OUT From suppressor regen out REGEN IN ELUENT IN CR-TC ELUENT OUT From pump Dionex Integrion Operator’s Manual Thermo Scientific...
Page 213 4. While holding the Dionex EGC with the ports on the bottom, tap the cartridge with the palm of your hand 10 to 15 times to dislodge air bubbles that may be trapped in the electrolysis chamber. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 214 Dionex EGC. The pump flow is on during flushing; however, no flow reaches the suppressor or Dionex CR-TC 600. 2. Set the pump flow to 1.0 mL/min and turn on the flow. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 215: Replacing A Dionex Cr-Tc 600
3. Unplug the Dionex CR-TC 600 cable (pull it straight out of the connector). 4. Disconnect the liquid lines from the four ports on the Dionex CR-TC 600. 5. Pull the Dionex CR-TC 600 straight off of its mounting location and remove it from the system. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 216 Dionex CR-TC 600, and then push the Dionex CR-TC 600 firmly onto the mounting ball studs. The CR-TC clicks into place when properly installed. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 217: Servicing High-Pressure (Injection) Valves
• 0.4 L Internal Loop High-Pressure Valve Maintenance Kit (P/N 075040) • 6-Port High-Pressure Valve Maintenance Kit (P/N 075974) • 10-Port High-Pressure Valve Maintenance Kit (P/N 079053) Note Substitution of non-Dionex/Thermo Fisher Scientific parts may impair valve performance and void the product warranty. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 218: Replacing A High-Pressure Valve Pod
2. Flip the power switch on the rear panel to turn off the system power. 3. Open the column compartment door. 4. Disconnect each liquid line connected to the valve. 5. Grasp the front of the valve pod and pull out firmly to remove it from the system. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 219: Servicing A Dionex Integrion Conductivity Detector
11. Close the door. Servicing a Dionex Integrion Conductivity Detector This section includes the following procedures: • “Calibrating a CD Cell” page 202 • “Replacing a CD” page 203 • “Replacing a Suppressor” page 204 Thermo Scientific Dionex Integrion Operator’s Manual...
Page 220: Calibrating A Cd Cell
3. After calibration, flush the KCl solution from the system by pumping ASTM Type I (18 megohm-cm) filtered and deionized water through the cell. When the conductivity drops to less than 1 S/cm, stop the pump. 4. Reconnect the system plumbing for routine operation. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 221: Replacing A Cd
Air bubbles in the cell can cause pulsations of the baseline, random noise, and low readings. Air may result from outgassing of the eluent. Items needed • Standard disposable laboratory gloves (powder-free, particle-free, and oil-free) • Protective eyewear Thermo Scientific Dionex Integrion Operator’s Manual...
Page 222: Replacing A Suppressor
Refer to the suppressor manual for guidance about when to replace a suppressor and for instructions on how to prepare a new suppressor before initial use. Suppressor manuals are provided on the Thermo Scientific Reference Library DVD (P/N 60-053891). Items needed •...
Page 223: Servicing A Dionex Integrion Electrochemical Detector
4. Disconnect the cell outlet and inlet lines from the ED cell and disconnect the two electrical cables. 5. Grasp the cell by the cell body and pull straight out to remove it from the detector. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 224: Replacing An Ed
For installation instructions for disposable working electrodes, refer to the installation guide shipped with the electrodes (listed below) or to Product Manual for Disposable Electrodes (Document No. 065040), which is provided on the Thermo Scientific Reference Library DVD (P/N 60-053891).
Page 225: Replacing A Conventional Working Electrode Gasket
Note Handle the cell gasket and the inside surfaces of the cell carefully to prevent scratches, which may subsequently cause leaks. 3. Squeeze the tabs on the sides of the yoke block and pull the block and knob off the working electrode (see Figure 95). Thermo Scientific Dionex Integrion Operator’s Manual...
Page 226 1. Orient the cell assembly with the yoke knob on the left and then push the cell onto its mounting location on the ED. 2. Reconnect the cell inlet and outlet lines. 3. Reconnect the two electrical cables. 4. Start the pump flow. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 227: Polishing A Conventional Working Electrode
Designate a pad that will not be used with polishing compound. This pad is for removal of particles after polishing (see Step Thermo Scientific Dionex Integrion Operator’s Manual...
Page 228 Note It is not possible to over tighten the yoke knob. Once the knob clicks into place, it does not tighten any further. The yoke knob ensures constant pressure is applied to the cell. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 229: Replacing A Ph-Ag/Agcl Reference Electrode
Table 34. Recommended pH buffer solutions Product Quantity Fisher Scientific P/N pH 4 Calibration and Check Standard 500 mL SB101-500 pH 7 Calibration and Check Standard 500 mL SB107-500 pH 10 Calibration and Check Standard 500 mL SB141-500 Thermo Scientific Dionex Integrion Operator’s Manual...
Page 230 2. Hold the electrode vertically, with the cable up and the storage cap down, to prevent spilling the storage fluid in the cap. Unscrew the storage cap from the electrode. Be careful not to spill the contents. Save the cap. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 231 2. Verify that the O-ring is present on the pH-Ag/AgCl reference electrode (see Figure 99). Figure 99. pH-Ag/AgCl reference electrode O-ring pH-Ag/AgCl reference electrode O-ring Thermo Scientific Dionex Integrion Operator’s Manual...
Page 232: Replacing A Pdh Reference Electrode
• The PdH reference electrode typically lasts several years, depending on use. Items Needed • PdH reference electrode (P/N 072075) • O-ring (P/N 030839) • Wrench • Tweezers • Standard disposable laboratory gloves (powder-free, particle-free, and oil-free) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 233 (see Figure 101). Figure 101. Removal of the PdH reference electrode nut 3. Pull the reference electrode out of the well (see Figure 102). Figure 102. Removal of the PdH reference electrode Thermo Scientific Dionex Integrion Operator’s Manual...
Page 234 9. A fitting with knobs is installed on the end of the PdH reference electrode. Align the knobs on the fitting with the grooves in the reference electrode well (see Figure 105). Dionex Integrion Operator’s Manual Thermo Scientific...
Page 235 5. Select DC Amperometry mode, set the DC voltage to 0.000 V, and turn on the cell voltage. Switch to mode, click Set Integrated Amperometry, Integrated Amperometry and select the Gold, PdH RE, Carbo, Quad waveform. 6. Condition the electrode for 1 hour at these settings. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 236: Changing The Main Power Fuses
Steckdose zu verwenden. Das Gerät darf nicht ohne Erdung betrieben bzw. an Wechselstrom angeschlossen werden. VORSICHT HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des Dionex Integrion. Dionex Integrion Operator’s Manual Thermo Scientific...
Page 237 5. Replace the two fuses with new 5 A, 250 V, 5 x 20 mm IEC 60127-2 fast-blow fuses (P/N 00006-03-00016). Thermo Fisher Scientific recommends always replacing both fuses. 6. Reinstall the fuse holder. Reconnect the power cord and turn on the power. Thermo Scientific Dionex Integrion Operator’s Manual...
Page 238 Service Changing the Main Power Fuses Dionex Integrion Operator’s Manual Thermo Scientific...
Page 239: Appendix A Specifications
Electrolytic eluent generation at high pressure 0.1–100 mM Gradient Profiles Any combination of an unlimited number of linear, convex, and concave positive and negative gradient profiles Eluent Shutoff Valve Electrically-actuated Leak Sensor Built-in, optical Thermo Scientific Dionex Integrion Operator’s Manual...
Page 240 Temperature Accuracy ±0.5 °C (at 15 °C) Temperature Stability ±0.2 °C (at 15 °C) Suppression Modes Electrolytic Suppression, Self-Regenerating, Recycle Mode Electrolytic Suppression, Self-Regenerating, External Water Mode Non-Suppressed Conductivity Supported (both anion and cation) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 241 Microprocessor-controlled digital signal processing Electronic Noise (Wet Noise) IPAD (Au electrode) < 50 pC at 10 mM KOH DC Amperometry (GC) < 10 pA at catecholamine eluent Potential Range -2.0 to 2.0 V in 0.001 V increments Thermo Scientific Dionex Integrion Operator’s Manual...
Page 242 USB Communication Protocol One USB input; one built-in two-output USB hub Dimensions (h × w × d) 62. 5 x 30 x 55.9 cm (24.6 x 11.8 x 22 in) Weight 41 kg (90 lb) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 243: Appendix B Reordering Information
Membrane (Part cannot be replaced by user) 60-078499 Seal wash seal insertion tool Seal Wash System 22153-62010 Seal Wash Pump Kit Eluent Reservoirs and Accessories 062510 Eluent reservoir, 2 liter 063292 Eluent reservoir, 4 liter 078520 Regulator Kit Thermo Scientific Dionex Integrion Operator’s Manual...
Page 244 High-pressure valve rebuild kit, 10-port Sample loop, 10 L 042949 Sample loop, 25 L 042857 079848 Low-pressure valve, 2-way 061971 Low-pressure valve, 3-way Detectors and Detector Cells 22153-62034 Dionex Integrion Conductivity Detector (with shipping container) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 245 Gasket for disposable working electrodes, PTFE, 0.001 in (2 gaskets) 062158 ED cell polypropylene support block (for use with disposable electrodes) 036313 Polishing kit for conventional working electrodes 036319 Coarse polishing compound 036318 Fine polishing compound Thermo Scientific Dionex Integrion Operator’s Manual...
Page 246 Viper assembly (RFIC systems), 0.18 mm (0.007 in), 178 mm (7.0 in) 088810 Viper assembly, 0.18 mm (0.007 in), 229 mm (9.0 in) 088811 Viper assembly, 0.18 mm (0.007 in), 241 mm (9.5 in) Dionex Integrion Operator’s Manual Thermo Scientific...
Page 247 924133 Connector plug, 8-position 923686 Connector plug, 12-position Maintenance Kit 22153-62041 Dionex Integrion HPIC System Preventive Maintenance Kit Miscellaneous Items 960777 USB cable (for PC), 1.8 m (6 ft) 00302-99-00119 USB cable (for mobile device), 16.5 cm (6.5 in) 22153-40107...
Page 248 Reordering Information Dionex Integrion Operator’s Manual Thermo Scientific...
Page 249 Analog-to-digital converter USB connections Analyses Virtual Column Separation Simulator Audit trail Column, trap Icons Command window Autosampler Commands Injecting samples Creating a program Loading samples Compartment temperature control Autozero compliance WEEE Concentration of eluent Thermo Scientific Dionex Integrion Operator’s Manual...
Page 250 Response range Electrochemical Detector (ED) Fuses Detection modes Replacement procedure ED cell description ED replacement procedure Operating Gas regulator Operating modes Glassy carbon electrodes Palladium hydrogen (PdH) reference electrode Gold electrodes pH-Ag/AgCl reference electrode Waveforms Dionex Integrion Operator’s Manual Thermo Scientific...
Page 251 Analog output Methanesulfonic acid eluent (MSA) 58–59 Potassium hydroxide eluent Methanol Power output Mobile app operation Power receptacle Using with Chromeleon Power switch (rear panel) Monitoring background Powering up the system Pressure limit tripped Thermo Scientific Dionex Integrion Operator’s Manual...
Page 252 Syringe Reproducibility is poor Manual injections 55–56 Reservoirs Using to prime pump Cleaning 159, 161, 165, System flow descriptions End-line filters System power-up Pressurizing System shutdown Setting up Reversed-phase solvents RFID Technical Support 109, Dionex Integrion Operator’s Manual Thermo Scientific...
Page 253 USB cable USB connections Troubleshooting Vacuum degasser Vacuum is low Valves 4-port high-pressure (injection) Injection Low-pressure Rebuilding high-pressure valves Replacing a high-pressure valve pod Virtual Column Separation Simulator Waste lines Water dip Water samples Waveforms Thermo Scientific Dionex Integrion Operator’s Manual...
Page 254 Index: Z Dionex Integrion Operator’s Manual Thermo Scientific...

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