ACQUITY UPLC HT Column Heater Instructions...ACQUITY UPLC HT Column Heater Instructions 7 Applying the thermal gasket: 3. Press the thermal gasket into the tray. Ensure that the gasket

ACQUITY UPLC HT Column Heater Instructions

Note: This document is an addendum to Revision C of the ACQUITY UPLC System Operator’s Guide.

OverviewWhen installed on Waters® ACQUITY UPLC® Systems, the Waters ACQUITY UPLC High Temperature (HT) Column Heater maintains one column at a temperature up to 90 ºC (194 ºF). The HT column heater is an assembly that fits on top of the sample manager and contains the column stabilizer assembly, the optional column in-line filter unit, and a column. The HT column heater’s front compartment can accommodate any Waters ACQUITY column up to 4.6 mm ID and 150 mm long. The column rests in a U-shaped tray, which swivels outward to any position between 0° and 180° and can receive the column from either side. Thus, in the 0°, “home”, position, the tray is directly above the sample manager and below the optical detector, and in the 180°, “away”, position, you can plumb the HT column heater into a mass spectrometer (located on the system’s right).

Contents:

Topic PageOverview 1Connecting the cable 4Installing the column stabilizer assembly 5Installing the column in-line filter 9Installing the column 10Installing the column in an MS system 13Maintenance 13Troubleshooting 19Specifications 20

71500148606, Rev. AACQUITY UPLC and Waters are registered trademarks, and eCord is a trademark of Waters

Corporation. PEEK tubing is a registered trademark of Victrex Corporation. Phillips is aregistered trademark of Phillips Screw Co.

All other trademarks are the sole property of their respective owners.Copyright © 2007 Waters Corporation.

ACQUITY UPLC HT Column Heater Instructions 1

The HT column heater uses an element of insulated film to heat the column compartment to any temperature between 5 ºC (9 ºF) above ambient and 90 ºC (194 ºF). A passive column stabilizer and thermal gasket inside the tray reduce sensitivity to ambient temperature swings and minimize bandspreading. A port on the HT column heater’s right-hand side receives the column’s eCord™ chip. The eCord stores column information, which you can access from the ACQUITY UPLC console.The HT column heater drip tray captures any leakage, routing it to the sample manager via a drip tube. If a leak sensor is fitted on the instrument and it is activated, a message appears in the Status area of the ACQUITY UPLC console, notifying you of the leak. At the rear of the HT column heater, a network switch offers seven Ethernet ports to connect the ACQUITY UPLC instruments to the system. See also: ACQUITY UPLC Online Help and ACQUITY UPLC System Operator’s Guide (part number 71500082502).

Requirements

• Empower, Empower 2, or MassLynx 4.1 or later data application • ACQUITY UPLC Console • Waters ICOP v.1.23 or later for sample manager (ACQ-SM) • Sample manager or autosampler for v.1.3 or later

Safety considerations

Observe these warning and caution advisories when you perform installation, maintenance, or troubleshooting tasks.

Warning: To avoid electric shock• power-off the sample manager before you connect or disconnect the

external communication cable (between the sample manager and the HT column heater). In addition, if the sample manager is powered-on when you connect the cable, the sample manager will sustain damage.

• do not open the HT column heater’s top cover. The HT column heater does not contain user-serviceable components.

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Warning: To avoid electric shock • power-off and unplug the HT column heater before performing any

maintenance on the instrument or making any electrical connections.

• use power cord SVT-type in the United States and HAR-type or better in Europe. For other countries, contact your local Waters distributor.

• connect the HT column heater to a common ground.

Warning: To prevent burn injuries, set the column temperature to Off, and then allow the column compartment and its components to cool for 60 minutes before touching them. Monitor the column compartment internal temperature to ensure all components are cool.

Warning: To prevent injury and avoid possible exposure when working with hazardous solvents• install the system in a hooded environment.• ensure that the lab environment has a sufficient rate of air

exchange. • using incompatible solvents can cause severe damage to the

instrument and/or injury to the operator. • to avoid possible exposure to hazardous solvents, do not remove the

drip tray.

Warning: To prevent injury, always observe Good Laboratory Practices when you handle solvents, change tubing, or operate the system. Review the Material Safety Data Sheets for the solvents in use so that you know their physical and chemical properties.

Warning: Fire and explosion hazard. Do not use any solvents whose auto-ignition temperatures are below 105 ºC (221 ºF).


Requirement: To obtain accurate, reproducible chromatograms, use only MS-grade solvents, water, and additives. For details, see Appendix D of the Waters ACQUITY UPLC System Operator’s Guide.

Connecting the cableThe sample manager powers and communicates with the HT column heater. The external communication cable must be connected to the rear of the HT column heater and the sample manager.

1. Make sure the sample manager and the HT column heater are powered-off.

2. Connect the external communication cable to the High Density (HD) port on the rear of the HT column heater.

3. Connect the other end of the external communication cable to the QSPI port on the rear of the sample manager.

Caution: • To avoid damaging electrical parts, never disconnect an electrical

assembly while power is applied to an instrument. To completely interrupt power to an instrument, set the power switch to Off, and then unplug the instrument’s power cord from the AC outlet. After power is removed, wait 10 seconds before you disconnect an assembly.

• To prevent circuit damage because of static charges, do not touch integrated circuit chips or other system components that do not require manual adjustment.

• To avoid damaging the HT column heater, the weight of items stacked on top of it should not exceed 18.1 kg (40 pounds).

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Connecting the external cable:

Installing the column stabilizer assemblySee also: “Replacing the column stabilizer assembly” on page 18.

Required materials

• Phillips® screwdriver • High-temperature outlet fitting wrench• 5/16” open-end wrench


Rear of sample manager

Rear of HT column heater

CH external communication cable

ETHERNET

High Density Connector

Fuses and power connection

RS-232(A)

RS-232(B)

ETHERNET

QSPI

I II


• Column stabilizer kit (part number 205000489 for 50- or 100-mm column, or 205000494 for 150-mm column): – Column stabilizer assembly– Collet and compression screw multi-tool (collet separator)– 3 Phillips screws (1 is a spare)– 3 thermal gaskets (2 are spares)

– PEEK® tubing for connecting the column to the detector’s flow cell

To install the column stabilizer assembly:

1. Open the HT column heater door, lift up and rotate the metal latch clockwise, and tilt the column heater tray 45 degrees downward.

Opening the column heater tray:

2. Remove the clear, protective backing from the thermal gasket, and with the thermal gasket oriented vertically, center it between the two threaded holes.

Column heater tray Metal latch

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Applying the thermal gasket:

3. Press the thermal gasket into the tray. Ensure that the gasket is centered and formed into the bottom of the tray with equal lengths on both sides.

4. With the inlet tubing on the right, firmly press the column stabilizer assembly into the thermal gasket. Ensure that the thermal gasket uniformly envelops the sides of the column stabilizer and does not bunch beneath it.

Column stabilizer assembly (two styles):

Thermal gasket

Threaded holes

TP02544

Reusable fittings

Inlet tubing to injector

For 150-mm column

For 50-mm or 100-mm column


Installing the column stabilizer assembly:

5. Carefully route the column stabilizer inlet tubing through the groove on the right-hand side of the tray.

6. Insert two Phillips screws into the threaded holes, and tighten them gently using the Phillips screwdriver.

7. Remove the O-ring retainer from the inlet end of the column stabilizer tube, and then connect the inlet tube to injector port 6 of the sample manager.

Caution: To avoid stripping the threads, do not overtighten screws.

TP02845

Column stabilizer inlet tubing

Threaded holes for Phillips screws

Thermal gasket visible along both sides of

stabilizer

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Connecting to the injector:

Installing the column in-line filterSee also: “Replacing the filter or the column in-line filter unit” on page 16.

To install the column in-line filter:

1. Remove the O-ring retainer from the outlet end of the column stabilizer tube. Tip: Before connecting, make sure that the ferrule is approximately 3 mm from the end of the outlet tube and that the collet is touching the back of the ferrule.

Positioning the fitting on the column stabilizer outlet tube:

Caution: To prevent contamination, wear powder-free, non-latex gloves when connecting tubing and tightening fittings.

Port 6 of injector

Inlet tubing of column stabilizer

Reusable fitting Ferrule

3 mm Collet

Outlet tube


2. Remove the column in-line filter unit from its packaging, and then push the outlet end of the column stabilizer tubing assembly into the in-line filter inlet until it stops.

Connecting the in-line filter unit:

3. Holding the reusable fitting in place, rotate the in-line filter unit onto the fitting until it is snug.

4. Finger-tighten the fitting until it is snug, and then add a quarter-turn.

Installing the columnSee also: “Replacing the column” on page 15.

To connect the column in-line filter unit and the column inlet:

1. Remove the O-ring from the outlet end of the column in-line filter unit.

2. Remove the plug from the column inlet.

3. Push the outlet end of the column in-line filter unit into the column inlet until it stops.

4. Tighten the fitting until it is snug, and then add a quarter-turn.

Caution: To avoid damaging the tubing, use only your fingers to tighten the tubing fittings.

Caution: To avoid damaging the tubing, use only your fingers to tighten the fittings.

Flow

In-line filter unit Column Column stabilizer tubing assembly

Inlet Reusable fitting

10

To install the PEEK tubing in the column outlet:

1. Insert the PEEK tubing into the high-temperature outlet fitting until it stops.

2. Holding the PEEK tubing, thread the high-temperature outlet fitting into the column outlet (to the right) until it is finger-tight.

3. Using a 5/16” wrench to hold the column steady, use the high-temperature outlet fitting wrench to give the outlet fitting a quarter turn.

4. Push the PEEK tubing into the left-hand side of the column tray.

To connect the PEEK tubing to the detector:

1. Remove the protective cover from the PEEK tubing from the flow cell inlet in the detector.

2. Attach the 0.0625-inch OD inlet tubing (included with the flow cell or the stabilizer kit) to the column outlet. Check the label on the flow cell inlet tubing to ensure it matches the type of detector and flow cell in your system.

Connecting the column to a flow cell:

Caution: To avoid bandspreading, ensure that the tubing is fully bottomed in the fitting hole before tightening it.

Caution: To avoid damaging the outlet fitting, do not over-tighten it with the outlet fitting wrench.

TP02401Detector inlet tubing (PEEK) from column

Detector flow cell assembly

Outlet

Inlet


3. Snap the column support clips onto the body of the column (one between the reusable fitting and column). Rotate the clips so that the openings face forward.

4. Place the column in the tray.

5. Close the column heater tray, and then push down the metal latch to secure the column stabilizer tubing.

6. Close the HT column heater door, and then inspect the seal around the front panel to ensure it aligns correctly. Note: Proper alignment of the seal is critical for a stable thermal environment.

7. Attach the eCord fob to the receptacle on the right-hand side of the HT column heater.

Connecting the eCord:

Requirement: The external communication cable must be connected to the HD port on the rear of the HT column heater and the QSPI port on the rear of the sample manager, so that the sample manager can power and communicate with the HT column heater.

8. Power-on the sample manager and the remaining ACQUITY UPLC instruments.

Warning: To avoid electric shock or possible damage to the components, power-off the sample manager before you connect or disconnect the external communication cable (between the sample manager and the HT column heater).

eCord receptacleeCord fob

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Setting the column temperature

To set the temperature:

1. In the Empower Run Samples window, click Instrument method editor > View Method tab. Alternative: MassLynx main window > Instrument tab > Inlet Method.

2. Click ACQ-SM (Empower) or Autosampler (MassLynx).

3. Specify a value between “ambient plus 5 °C” and 90 °C. Alternative: Select Off to keep the column at ambient temperature. Tip: The HT column heater does not have cooling capabilities. The lowest temperature is 5 degrees above ambient temperature.

4. Click OK (for MassLynx only).

5. Allow the column to warm. In the Plots area of the ACQUITY UPLC Console, monitor temperatures to ensure that the system is thermally equilibrated.

Installing the column in an MS systemIf your system includes a mass spectrometer positioned to the right of the system stack, open the HT column heater door in the “away” position (swinging rightward) to connect to the MS inlet without increasing the tubing length. The MS drip tray is required to ensure any solvent leaked from the column or column connections is routed into the drip management system. See also: chapter 2 of the Waters ACQUITY UPLC System Operator’s Guide to replace or install the column, in-line filter, and column stabilizer assembly in a HT column heater for MS detection.

MaintenanceWaters recommends that you perform routine maintenance to ensure reliable operation and accurate results. When using the system throughout the day (and on nights and weekends), or when using aggressive solvents such as buffers, perform maintenance tasks more frequently.


Spare parts

You can replace the column, the column stabilizer assembly, the column in-line filter unit, and the filter.

See also: www.waters.com for information on columns.

Recommended maintenance schedule:

Maintenance procedure Frequency For information...Replacing the filter in the column in-line filter unit

During scheduled preventive maintenance

See page 16.

Replacing the column in-line filter unit

After you use the six filters that accompany the filter unit

See page 9.

Replacing the column stabilizer assembly

As needed See page 5.

Replacing the column As needed See page 15.

Caution: Waters does not recommend you replace parts that are not listed as spare parts.

Recommended spare parts:

Item Part NumberColumn stabilizer assembly 205000489Column stabilizer assembly, 150-mm column 205000494 Column in-line filter unit 205000343Replacement filters 700002775

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Maintaining the HT column heater

Under normal operating conditions, the HT column heater does not require routine maintenance. If residue from solvent leaks accumulates in the tray, remove the column, and wipe the tray clean with a soft cloth.

Replacing the column

Requirement: Stop any currently running mobile phase before replacing the column.

To remove the column:

1. After cooling, open the HT column heater door.

2. Disconnect the stabilizer outlet tube from the column or in-line filter.

3. Place the forked end of the collet separator over the collet on the column stabilizer tube, and gently wiggle it back and forth to pry the reusable fitting loose from the collet.

Warning: To avoid electric shock or possible damage to the components, power-off the sample manager before you connect or disconnect the external communication cable (between the sample manager and the HT column heater).

Warning: To avoid possible exposure to hazardous solvents, do not remove the tray.

Warning: To prevent burn injuries, set the column temperature to Off, and then allow the column compartment and its components to cool for 60 minutes before touching them. Monitor the column compartment’s internal temperature to ensure all components are cool.

Caution: To prevent contamination, wear powder-free, non-latex gloves when replacing the column.


Disassembling the reusable fitting:

4. Replace the ferrule.

5. Continue with “Installing the column” on page 10.

Replacing the filter or the column in-line filter unit

Recommendations: • To minimize wear on the compression fittings, replace the in-line filter

unit only after you use the six filters that accompany the unit.• The column in-line filter unit cannot completely prevent or reverse

system contamination. You should therefore try to prevent contamination and troubleshoot it when it occurs, as well as clean or replace contaminated components.

See also: “Controlling Contamination in Ultra Performance LC®/MS and HPLC/MS Systems” (part number 715001307). Requirement: Stop any currently running mobile phase before replacing the filter.

Caution: To prevent contamination, wear powder-free, non-latex gloves when replacing the filter.


Collet separator

Reusable fitting

Tubing from injector

Ferrule

Collet

16

Required materials

• Open-end wrenches, 5/16-inch (2)• Powder-free, non-latex gloves• Replacement filter or column in-line filter unit

To replace the filter or the column in-line filter unit:

1. Open the column heater door, lift up the metal latch, and tilt the column heater tray downward.

Opening the column heater tray:

2. Pull out the column and in-line filter unit from the tray so that you can access the in-line filter unit.

3. Disconnect the column stabilizer tubing assembly from the in-line filter unit.

4. To replace the in-line filter unit, detach it from the column inlet, attach a new unit in its place, and continue with step 8.

5. To replace the filter, open the in-line filter unit by placing two 5/16-inch open-end wrenches onto the flats. Do not detach the unit from the column inlet.

Column heater tray Metal latch


Disassembling and assembling the in-line filter unit:

6. From the in-line filter unit, remove the inlet nut that contains the used filter. Note: Discard the used filter; it cannot be used again.

7. Insert a new filter, and then reassemble the in-line filter unit.

8. Start the mobile phase flowing.

9. Examine the components for leaks, tightening fittings as needed.

10. Place the assembled components into the column tray, push down the metal latch to secure the tubing, and tilt the tray upward to the closed position.

Replacing the column stabilizer assembly

Requirement: Stop any currently running mobile phase before replacing the column stabilizer assembly.


Caution: To prevent contamination, wear powder-free, non-latex gloves when replacing the column stabilizer assembly.

TP02543

Outlet assembly Filter Inlet nut

Flow

Place wrenches on flats to assemble and disassemble.

18

To replace the column stabilizer assembly:

1. Disconnect the inlet tube from injector port 6 of the sample manager.

2. Open the door.

3. Using the Phillips screwdriver, loosen the two screws that fasten the column stabilizer assembly to the tray.

4. Remove the column stabilizer assembly from the thermal gasket.

5. Using the 1/4-inch and 5/16-inch open-end wrenches, disconnect the compression fitting that attaches the column stabilizer assembly to the optional in-line filter or to the column.

6. Continue with “Installing the column stabilizer assembly” on page 5.

Troubleshooting

Warning: To avoid electric shock or possible damage to the components, power-off the sample manager before you connect or disconnect the external communication cable between the sample manager and the HT column heater.

Symptom SolutionAn error message about the HT column heater appears.

See ACQUITY UPLC online help.

The HT column heater or sample manager loses power or fails to power-on, or status LEDs are unlit.

Replace the fuse in the sample manager. The sample manager powers the HT column heater.

You must monitor column history, determine column status, or clean, regenerate, or equilibrate a column.

See chapter 7 in the ACQUITY UPLC System Operator’s Guide and ACQUITY UPLC online help.


Specifications

You must install reusable fittings. See “Installing Finger-tight Reusable Fittings (Column Heater)”, available in the Waters Support Center (www.waters.com).

You suspect contamination. See “Controlling Contamination in Ultra Performance LC®/MS and HPLC/MS Systems” (part number 715001307).

Environmental specifications:

Attribute SpecificationOperating temperature 4 to 40 °C (39.2 to 104 °F)Operating humidity <95%, noncondensingShipping and storage temperature −30 to 60 °C (−22 to 140 °F)Shipping and storage humidity 20 to 85%, noncondensingAcoustic noise (instrument generated)

<50 dBA

Temperature control within the range of 20 °C (or ambient plus 5 °C, whichever is higher) to 90 °C, settable in 0.1 °C increments

Temperature precision ± 0.1 °C after a resetTemperature accuracy ± 1 °C Temperature distribution ± 3 °C up to 65 °C

± 5 °C above 65 °C

Symptom Solution

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Documents

ACQUITY UPLC HT Column Heater Instructions...ACQUITY UPLC HT Column Heater Instructions 7 Applying the thermal gasket: 3. Press the thermal gasket into the tray. Ensure that the gasket