Configuring the Dionex Integrion HPIC

Te ch ni cal N ote 1 7 5
System for High-Pressure Reagent-Free Ion
Chromatography
Terri Christison, Jingli Hu, David Moore, Linda Lopez, Jeff Rohrer
Thermo Fisher Scientific, Sunnyvale, CA

Key Words
Standard Bore, Fast IC, IonPac AS19-4µm column,
IonPac AS18-4µm column, IonPac AS19 column, Reagent-Free IC

Goal
Provide installation instructions to install a Reagent-Free™ IC application
using standard bore columns on the Thermo Scientific™ Dionex™ Integrion™
HPIC™ system.

Introduction
The latest advancement in ion chromatography (IC)
instrumentation, the high-pressure Thermo Scientific™
Dionex™ Integrion™ HPIC™ system, can operate
continuously up to 5000 psi for both 4 mm and 2 mm
i.d. column formats when using automated eluent
generation. The Dionex Integrion HPIC system can
therefore take advantage of the high-efficiency separations
• Components are tracked by consumables device
offered by smaller-particle-size separation columns. When
tracking technologies for GMP compliance tracking and
combined with the advantages and ease-of-use of
to assure installation of compatible devices
Reagent-Free™ IC (RFIC™), this system provides enhanced
resolution of closely eluting peaks with excellent • Independent tablet control for convenient, continuous
reproducibility, thereby yielding greater quantification chromatography monitoring, independent manual
accuracy and consistently reliable results. control, and access to the instrument manual and
troubleshooting guides
The Dionex Integrion HPIC system, configured for
• New Thermo Scientific™ Dionex™ Chromeleon™ 7
Reagent-Free IC with suppressed conductivity detection,
Chromatography Data System (CDS) software features
includes many of the recent advancements in IC
provide easy instrument configuration, monitoring of
instrument technology, including high-pressure
consumable devices, and integrated video instructions
capabilities, Reagent-Free IC (RFIC) consumables for
for conditioning columns, suppressors, and other
inline eluent generation, column heater control, and new
electrolytic devices
features designed to make the system easier to use:
In this technical note, we provide installation
• Compact, fully integrated system design recommendations for a Dionex Integrion HPIC system
• Easy access to eluent generator cartridge and configured for analytical flow rates (0.10–2.0 mL/min)
electrolytic trap column using electrolytically generated eluents. Results will
• Separate compartments for pump, column heater with highlight some of the instrument, column, and suppressor
injection valve, and detector with suppressor to provide features.
faster column oven equilibration and to extend
temperature control to suppressors
• Thermo Scientific™ Dionex™ IC PEEK Viper™ fittings
replace standard fitting connections in specified
positions to minimize void volume problems, improving
chromatography and ensuring accurate reporting
2 Equipment
• Thermo Scientific Dionex Integrion HPIC high-pressure
IC system, including:
– Eluent Generation Capabilities
– CD Conductivity Detector
– Column Oven Temperature Control
– Detector-Suppressor Compartment Temperature
Control
– Tablet Control
• Thermo Scientific™ Dionex™ AS-AP Autosampler with
10 mL vial trays
Software
Thermo Scientific Dionex Chromeleon CM 7.2 SR4 CDS
software.

Table 1 lists the consumable products recommended for

the Dionex Integrion HPIC system configured for
suppressed conductivity detection.

Table 1. Consumables for the Dionex Integrion HPIC system.

Product Name High-Pressure Device Part Number

Dionex IC PEEK Viper Fitting Dionex IC PEEK Viper fitting assembly kit for the Integrion HPIC system using
088798
Tubing Assembly Kits conductivity detection: Includes one each of P/Ns: 088805 through 088811
Guard outlet to separator column: 0.007 × 4.0 in (102 mm) 088805
Injection Valve, Port C (Port 2) to guard column: 0.007 × 5.5 in (140 mm) 088806
Dionex IC PEEK Viper Fitting EGC Eluent Out to CR-TC Eluent In: 0.007 × 6.5 in (165 mm) 088807
Tubing Assemblies, Included
in Kit, P/N 088798 Separator to Suppressor Eluent In: 0.007 × 7.0 in (178 mm) 088808
Suppressor Eluent Out to CD In: 0.007 × 9.0 in (229 mm) 088810
CR-TC Eluent Out to Degasser In: 0.007 × 9.5 in (241 mm) 088811
Dionex AS-AP Autosampler Package of 100, polystyrene vials, caps, blue septa, 10 mL
074228
Vials
Thermo Scientific™ Dionex™ Eluent generator cartridge recommended for anion applications using
EGC™ 500 KOH Eluent 4 µm particle resin columns 075778
Generator Cartridge
Thermo Scientific™ Dionex™ Continuously regenerated trap column used with Dionex EGC KOH
CR-ATC™ 600 Electrolytic 500 cartridge 088662
Trap Column
HP EG Degasser Module Degasser installed after Dionex CR-TC trap column and before the Injection
075522
Valve. Used with eluent generation
Thermo Scientific™ Dionex™ Suppressor for 4 mm and 5 mm columns, using recycle mode
082540
AERS™ 500 Suppressor
Thermo Scientific™ Dionex™ For the applications shown in Figures 9 (Chromatogram B), 10, and 11:
IonPac™ AG18-4µm Column Anion guard column, 4 × 30 mm 076035

Dionex IonPac For the applications shown in Figures 9 (Chromatogram B), 10, and 11:
076034
AS18-4µm Column Anion separation column, 4 × 150 mm
Dionex IonPac For the application shown in Figure 12: Anion guard column, 4 × 50 mm
083221
AG19-4µm Column
Dionex IonPac For the application shown in Figure 12: Anion separation column,
083217
AS19-4µm Column 4 × 250 mm
Thermo Scientific™ Syringe filters, 25 mm, PES membrane, 0.2 µm. This syringe filter is Thermo
Nalgene™ Syringe Filter compatible with IC analysis. Scientific
7252520 /
Fisher Scientific
09-740-113
 3
Chromatographic Conditions
Dionex Integrion HPIC System
Columns Dionex IonPac columns, 4 mm i.d.
Fresh 18 M -cm
Eluent See chromatograms Resistivity
Deionized Water
Eluent Source Dionex EGC 500 KOH eluent cartridge, Dionex AS-AP Autosampler
Dionex Dionex
Dionex CR-ATC 600 and high-pressure Dionex EGC
500 cartridge
CR-TC Degas
600 trap Module
degas module Fresh 18 M -cm
Resistivity
Flow Rate See chromatograms Deionized Water
Pump Vent line

Column Temperature 30 °C
Injection Volume See chromatograms
Detection/Suppressor 15 °C
Waste
Compartment
Dionex ERS 500
Detection Suppressed conductivity, Dionex AERS suppressor CD

500 suppressor, 4 mm, recycle mode Dionex

IonPac
Run time See chromatograms Sample loop
Columns

Background Conductance < 1 µS

Figure 1. Flow diagram for the Dionex Integrion HPIC system.
Noise < 1 nS
Connect the USB cables from the IC system to the
System Backpressure Described in the Results section
autosampler and to the computer. Connect the power
cables and turn on the IC instrument and the autosampler.
Reagents and Standards
• 18 MΩ-cm resistivity degassed deionized (DI) water Configuring the Modules in the Chromeleon CDS
Software
• Thermo Scientific Dionex Combined Seven Anion
™ ™
To configure the IC system, first start the Dionex
Standard II, NIST traceable (P/N 057590)
Chromeleon Instrument Controller program and then
Instrument Setup and Installation select the link, Configure Instruments, to open the
The Dionex Integrion HPIC system is configured with a Chromeleon Instrument Configuration Manager.
CD Conductivity Detector with the intention to use eluent Right-click on computer name, select Add an Instrument,
generation and temperature control of the column oven and enter an appropriate name (for example: Integrion_
and detector-suppressor compartment. This system has EPA300_1). Add the following modules to this instrument
consumables device tracking through cable and radio configuration: Integrion HPIC System, Integrion
frequency, optional manual controls by the Dionex HPIC Pump Wellness, and Dionex AS-AP Autosampler.
Integrion HPIC system tablet, and can operate at
pressures up to 5000 psi with eluent generation. Integrion HPIC System Module
Select Add a Module, IC: Dionex Integrated Modules,
To set up this system, connect the Dionex AS-AP and Integrion HPIC System (Figure 2). The configuration
autosampler and the Dionex Integrion HPIC system for each module is summarized at the end of this section
according to Figure 1. Note that the injection valve is in Table 2.
plumbed through different ports than previous Dionex
IC systems.

Figure 2. Creating a configuration.

4 A window with multiple tabs will automatically open up Add the Dionex AS-AP Autosampler to the
(Figure 3). Select Model Serial No. in the General tab. The Configuration
Chromeleon CDS software will automatically detect all Add a new module by selecting the Dionex AS-AP
electrolytic devices, detectors (Figure 3), Pump Degasser, autosampler. Right-click on the module and select the
and Seal Wash (not shown). USB address. On the Segments/Pump Link tab, select the
appropriate vial trays for each color zone. On the Options
tab, select Push, installed syringe size, 1.2 mL for buffer
size, and enter the sample loop volume (Figure 5). Save
the configuration, select check the configuration, and then
close the Chromeleon Instrument Configuration program.

Figure 3. Automatic Detection of Electrolytic Devices.

Integrion HPIC Pump Wellness Module

To add pressure monitoring capabilities, it is necessary to
add another module: right-click and select Add a Module,
IC: Dionex Integrated Modules, Integrion HPIC Pump
Wellness module and then select a USB address to link the
module to the configuration. Select the Devices tab and
click on the Pressure Signal(s) box (Figure 4).

Figure 5. Configuring the AS-AP Autosampler.

Figure 4. Adding the Integrion HPIC Pump Wellness Module to the

Instrument Configuration.
As shown in Table 2, many of the devices are 5
automatically detected providing a fast, easy
configuration.

Table 2. Summary of the System Configuration for a Dionex Integrion HPIC system.

Tab Action Result

Integrion HPIC Module

General Link to USB address (Figure 2)
Pump - Flow rate and pressure limits are displayed
Detectors - Automatically detected
Electrolytics Automatically detects Dionex eluent generator cartridges and
-
Dionex CR-TC trap columns (Figure 3)
Inject Device - Automatically detected
Thermal Controls Automatically detects thermal control options for column, detector,
-
and suppressor
High-Pressure Valves - Automatically detected
Low-Pressure Valves - Automatically detected
Options - Automatically detects Pump Degasser and Seal Wash pump

Pump Wellness Module

Devices Check Pressure
Activates pressure monitoring feature (Figure 4)
Signal(s) box
Add Dionex AS-AP Autosampler
Add Module Link to USB
-
address
Sharing Only if more than one instrument is detected. If this option is present,
-
select Instrument
Segments / Pump Select 10 mL polystyrene vials or 1.5 mL vials for “Red”, “Blue”,
-
Link and “Green” (Figure 5)
Options Select Push, select syringe size, select 1.2 mL buffer line, enter the
-
loop size (Figure 5)
Finish Instrument Configuration
Check Configuration
Select Controller (On the top banner above the icons)

Select Check
Checks the configuration and reports errors.
Configuration
Save Select File, Save
Saves configuration
Installation
Close Close Instrument
Closes configuration program
Configuration file

Plumbing the Dionex Integrion HPIC System

First loosen the waste lines, including the metal-wrapped
waste line, in the back of the instrument and direct the
free ends to a waste container. To plumb the system,
first connect the pump eluent line to the eluent bottle
containing DI water previously degassed (vacuum
filtration and ultrasonic agitation). Prime the pump by
opening the priming knob ¼ turn and press the priming
button. Prime the pump until no bubbles are visible and
water is flowing at a steady rate out of the pump waste
line. Close priming knob to finger-tight. For more
information, review the Operator’s Manual1 by selecting
“?” on the tablet.
6 IC PEEK Viper Fittings Important: Do not remove consumables tracking device
Tip: To achieve the best chromatography, it is important tags from the columns or consumable devices. These tags
to gently tighten IC PEEK Viper fittings to finger-tight and are required for monitoring functionality.
to use the fitting assemblies in the following locations
Conditioning Electrolytic Devices and Columns
(Figure 6):
Install the Dionex EGC 500 KOH cartridge and Dionex
• Dionex EGC 500 KOH eluent generator cartridge CR-ATC 600 Continuously Regenerating Anion Trap
– Eluent Out to Eluent In on Dionex CR-ATC Column in the Integrion Reservoir Tray compartment.
600 trap column Condition the devices according to instructions in the
• Dionex CR-ATC 600 trap column – Eluent Out to Chromeleon Instrument Panel, drop-down menu
Eluent In on the Dionex Degas Module (Consumables, Install) (Figure 7). This information is also
available in the product manuals and the Dionex
• Injection Valve – “Column” port to the guard column
Integrion HPIC System Operator’s manual.1–3
• Between the guard and separation columns
To hydrate the Dionex ERS 500 suppressor, follow the
• Separation column to Eluent In on the Dionex AERS
QuickStart Instructions received with the suppressor and
500 Suppressor
also in the suppressor product manual.4 Wait for 20 min
• Dionex AERS 500 suppressor – Eluent Out to for the suppressor to fully hydrate before installing the
Eluent In on CD Conductivity Cell. suppressor in the Detector compartment. Install the black
IC PEEK Viper fittings (Figure 6) minimize void volume in PEEK (0.010 in i.d. tubing) backpressure loop from the
critical chromatography components, such as the columns slotted compartment next to the CD detector (exerting an
and suppressor. IC PEEK Viper fittings are also additional ~40 psi) between the CD outlet and the
recommended for use in consumable devices, such as the suppressor Regen In port.
eluent generator cartridge and trap column to minimize
Condition the columns for 30 min according to the
installation issues. The tubing is standard for both
instructions from the Consumables, Install Column
standard bore and microbore column applications.
section in the Chromeleon CDS software (Figure 7). The
The tubing length is specified for each connection (see
general practice is to use the eluent and flow rate
Table 1). The recommended practice is to tighten the
conditions listed in the QAR report while directing the
IC PEEK Viper fittings to finger-tight and then, if leaking
eluent exiting the column to a waste container.5,6
is observed, an additional 1/16 to 1/8 turn clockwise.
Complete the installation according to flow diagram in
Caution: Using a wrench or any other tool to tighten
Figure 1.
the IC PEEK Viper fittings may permanently damage
the fitting.

Figure 6. Dionex IC PEEK Viper fittings.

Figure 7. Consumables installation instructions on instrument panel.

Installing and Optimizing the Dionex AS-AP Set the eluent concentration, column oven, compartment 7
Autosampler oven, and cell temperatures as shown in the Conditions
For accurate injections and precise retention times, the section in the application. Allow the system to equilibrate
Dionex AS-AP autosampler needle must be aligned to the for 30 min.
injection port. To align the autosampler needle, first select
Creating an Instrument Method
the Sampler tab on the instrument panel, and press the
To create a new instrument method using the Chromeleon
Alignment button. Follow the commands to align the
Wizard, select Create, Instrument Method, and select an
autosampler needle to the Injection Port and Wash Port
Instrument. Enter the values from the Chromatographic
(Section B.12 in the Operator’s Manual).7 Connect the
Conditions section and those discussed under the
autosampler syringe line to the wash container containing
Dionex AS-AP section. Save the instrument method.
degassed DI water. Prime the syringe to flush out any air
in the Buffer Wash line and syringe. Initially select a Consumables Device Tracking
5000 µL wash volume until a steady flow of water is Tip: An action to either approve or correct an
observed at the Wash Port. Then, calibrate the transfer incompatibility between devices is required to start a
line volume by following the prompts on the TLV sequence after installing any new consumable device.
Calibration button. This volume will be recorded
A new feature of the Dionex Integrion HPIC system is
automatically. For more information, review Section 5.9
consumables device monitoring and tracking. This feature
in the Dionex IC Series AS-AP Autosampler Operator’s
automatically detects the electrolytic devices and the
Manual.7
columns. Review and approval of the devices is required
Starting the Dionex Integrion HPIC System to start the first sequence on the Dionex Integrion HPIC
To start the system, turn on the pump, and immediately system and when new consumable devices are installed.
turn on the Dionex EGC 500 eluent generator cartridge. To access this approval, select Consumables and then
Turn on the Dionex CR-ATC 600 trap and Dionex Inventory (Figure 8). The device monitoring shows the
AERS 500 suppressor when liquid is flowing through the device history, tracking: Part No., size, serial numbers,
devices. The system backpressure is dependent on the flow manufacture lot, installed location (On Device), and
rate and type of column, but the system pressure must be Best if Used by Date (Figure 8, top). Additionally,
above 2000 psi to support the Dionex EGC cartridges. the device monitoring will provide warnings if there
Typically, columns with 4 µm resin particles operate is incompatibility with the devices installed (Figure 8,
above 2000 psi and, therefore, do not require bottom left). To start the sequence, correct any errors,
backpressure tubing. However, if additional pressure is review the inventory, Approve, and Close the page
needed to achieve system pressures > 2000 psi, install (Figure 8, bottom right). Then select the Instrument
yellow PEEK backpressure tubing (yellow PEEK, Queue tab, and conduct a Ready Check on the sequence
0.076 mm i.d., 0.003 in i.d.) between the Dionex HP and Start.
Degas device and the injection port (Pump port position).

Figure 8. Consumables tracking.

8 Results and Discussion In the following environmental applications, inorganic
The determination of inorganic anions and oxyhalides anions were determined in wastewater and surface water
from disinfection processes in municipal drinking, waste, samples using the Dionex IonPac AS18-4µm columns
and bottled waters according to the U.S. EPA Methods (4 × 150 mm). Oxyhalides were determined in a bottled
300.0 (A) (B) and 300.1 (A) (B) are the most popular and water sample using the 2 × 250 mm, Dionex IonPac
widely used ion chromatography methods. AS19-4µm column.

The Dionex IonPac AS18-chemistry separation columns The analyses were facilitated by the Dionex Integrion
optimized for inorganic anion determinations are among HPIC system using the eluent generation and temperature
the latest innovations in hydroxide-eluent-optimized control of the both the column compartment and the
column chemistry. As such, there are many members of detector-suppressor compartment.
the Dionex IonPac AS18-chemistry family of columns:
In Figure 9, Chromatograms A and B compare the anion
• Three formats of the 250 mm length, 7.5 µm super separations of a standard on the 4 µm and 7.5 µm resin
macroporous resin particle columns (0.4 mm, 2 mm, particles formats, respectively of 4 × 150 mm (fast)
and 4 mm i.d.) for higher resolutions are needed for Dionex IonPac AS18 columns using the same conditions.
more complex samples In both examples, the anions were separated using an
• Three formats of the Dionex IonPac AS18-Fast, electrolytically generated hydroxide gradient from
150 mm length, with the same resin as the 250 mm 15 to 44 mM KOH at 1 mL/min and detected by
columns, for faster separations of well-defined samples suppressed conductivity within 9 min. As expected,
the smaller-particle-size column had increased peak
• Three formats of the Dionex IonPac AS18-4µm,
efficiencies, as evident in the smaller peak widths and
150 mm length, 4 µm super macroporous resin particle
higher peak response. The column pressure also increased
columns combining higher resolution with faster
as expected. In Chromatogram B, the system backpressure
separations
using the Dionex IonPac AS18-4µm column is
The Dionex IonPac AS19-chemistry high-capacity approximately 2600 psi, more than twice (~1100) that of
anion-exchange columns are optimized for oxyhalide the same system running the Dionex IonPac AS18-Fast
anion determinations but also suitable for inorganic anion column (Chromatogram A). The Dionex Integrion HPIC
determinations. These columns are available in three system brings high-pressure capabilities to the Integrated
formats (0.4 mm, 2 mm, and 4 mm i.d. by 250 mm) for systems for standard bore and microbore columns,
both the 7.5 µm super macroporous resin and the 4 µm thereby taking advantage of the 4 µm resin particle
super macroporous resin particles. columns.

Figure 9. Comparison of Dionex IonPac AS18 columns.

Fast anion determinations were demonstrated in a 9
five-fold diluted municipal wastewater sample (Figure 10)
and in an undiluted surface water sample (Figure 11)
using the Dionex IonPac AS18-4µm column. For more
information on analyzing environmental water samples
for common anions please see Application Update 200.8

Figure 10. Anions in a municipal wastewater sample.

Figure 11. Surface water sample.

For oxyhalide determinations, a large volume injection

is needed to achieve the ppb (µg/L) sensitivity required.
In Figure 12, µg/L concentrations of oxyhalides were
determined in a bottled water sample spiked with
oxyhalide standards using the high-resolution Dionex
IonPac AS19-4µm column. The top chromatogram is
rescaled to show the ppb concentrations of oxyhalides.
The lower chromatogram is at full scale. The system
backpressure is 3800 psi, which when using eluent
generation, can only be run on an HPIC system, including
a Dionex Integrion HPIC system.
 Te ch ni cal N ote 1 7 5
Figure 12. Bottled water sample with added oxyhalides.

Conclusion References
The installation and setup of the Dionex Integrion HPIC 1. Thermo Fisher Scientific. Dionex Integrion HPIC
system configured for eluent generation and suppressed System Operator’s Manual. P/N 22153-97003,
conductivity detection were discussed. Sunnyvale, CA, 2016.

The analysis of environmental water samples for 2. Thermo Fisher Scientific. Dionex Product Manual for
inorganic anions and oxyhalides was demonstrated using Eluent Generator Cartridges. P/N 065018-05,
electrolytically generated hydroxide eluents on different Sunnyvale, CA, June 2014.
column chemistries and formats: 3. Thermo Fisher Scientific. Dionex Product Manual for
the Continuously Regenerated Trap Column (CR-TC).
• The fast 4 × 150 mm Dionex IonPac AS18-Fast column
P/N 065018-05, Sunnyvale, CA, 2016.
with 7.5 µm resin particles
4. Thermo Fisher Scientific. Dionex ERS 500 Suppressor
• The fast 4 × 150 mm Dionex IonPac AS18-4µm column
Product Manual. P/N 031956-09, Sunnyvale, CA,
with 4 µm resin particles
November 2013.
• The high-capacity 2 × 250 mm Dionex IonPac
5. Thermo Fisher Scientific. IonPac AS18-4µm Column
AS19-4µm column with 4 µm resin particles
Product Manual. P/N 065499-02, Sunnyvale, CA,
The Dionex Integrion HPIC system, as shown in this August 2014.
configuration, has eluent generation, temperature control,
6. Thermo Fisher Scientific. IonPac AS19-4µm Column
easy access to consumables, high-pressure capability,
Product Manual. P/N 065532-02, Sunnyvale, CA,
consumables tracking, and low void volume IC PEEK
March 2014.
Viper fittings. Together these features provide a robust
easy-to-use system while taking advantage of new 7. Thermo Fisher Scientific. Dionex AS-AP Operator’s
technology advancements in IC consumable products. Manual. Document No. 065259, Sunnyvale, CA, 2012.
8. Thermo Scientific Application Update 200: Fast Anion
Determinations in Environmental Waters Using a High-
Pressure Compact Ion Chromatography System.
Sunnyvale, CA [Online] http://www.thermoscientific.com/
content/dam/tfs/ATG/CMD/cmd-documents/sci-res/app/
chrom/ic/sys/AU-200-IC-Inorganic-Anions-Environmental-
Waters-AU70922-EN.pdf (accessed Mar. 11, 2016).

www.thermofisher.com/chromatography
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