Teledyne Installation Guide Installation Manual

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CombiFlash® R

Installation Guide

For indoor use only

Phone: (402) 464-0231 Toll Free: (800) 228-4373 FAX: (402) 465-3022

Revision A: August 15, 2007

Part #60-5233-385

iii

CombiFlash® R

Installation Guide

Table of Contents

1. Introduction

1.1 Documentation Overview . . . . . . . . . . . . . . . . . . . . . .1-1

1.2 Product Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1

1.3 Operating Overview . . . . . . . . . . . . . . . . . . . . . . . . . .1-3

1.3.1 Multiple Control Possibilities . . . . . . . . . . . . .1-3

1.3.2 File Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3

1.4 Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4

1.5 Controls, Indicators, and Features . . . . . . . . . . . . . . 1-5

1.6 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8

1.6.1 Hazard Severity Levels . . . . . . . . . . . . . . . . . .1-9

1.6.2 Hazard Symbols . . . . . . . . . . . . . . . . . . . . . . . 1-10

1.7 For Additional Information . . . . . . . . . . . . . . . . . . .1-11

2. System Preparation

2.1 Unpacking the Unit . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

2.2 Instrument Location . . . . . . . . . . . . . . . . . . . . . . . . .2-1

2.3 Connect Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-2

2.4 Connect Solvent Lines . . . . . . . . . . . . . . . . . . . . . . . .2-2

2.5 Connect Waste Lines . . . . . . . . . . . . . . . . . . . . . . . . . 2-5

2.6 Optional External Gas . . . . . . . . . . . . . . . . . . . . . . . . 2-9

2.7 Connect and Route Drain Lines . . . . . . . . . . . . . . . .2-9

2.8 Position the System . . . . . . . . . . . . . . . . . . . . . . . . . .2-9

2.9 Install Collection Tube Racks . . . . . . . . . . . . . . . . .2-10

2.10 Turn on Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-12

2.11 Configure the System . . . . . . . . . . . . . . . . . . . . . . . . 2-12

2.11.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12

2.11.2 General Settings . . . . . . . . . . . . . . . . . . . . . . . 2-13

2.11.3 Vapor Limit . . . . . . . . . . . . . . . . . . . . . . . . . . .2-13

2.11.4 Automatically Print Report at End of Run . . 2-14

2.11.5 Enable Run Length Extension . . . . . . . . . . . .2-14

2.11.6 Set Default Tube Volumes . . . . . . . . . . . . . . . 2-15

2.11.7 Set Date/Time . . . . . . . . . . . . . . . . . . . . . . . . .2-15

2.11.8 Default Run Units . . . . . . . . . . . . . . . . . . . . .2-16

2.11.9 Gradient Method . . . . . . . . . . . . . . . . . . . . . .2-16

2.12 Prime the Solvent Lines . . . . . . . . . . . . . . . . . . . . . .2-17

CombiFlash® Rf Installation Guide

3. Operation

3.1 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.1 Liquid Sample Injection . . . . . . . . . . . . . . . . . 3-1

3.1.2 Solid Samples . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.3 Preloading on Column . . . . . . . . . . . . . . . . . . 3-3

3.2 Loading a RediSep R

Column . . . . . . . . . . . . . . . . . 3-3

3.3 Start a Default Method . . . . . . . . . . . . . . . . . . . . . . . 3-4

3.4 During the Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6

3.4.1 Run Control Buttons . . . . . . . . . . . . . . . . . . . . 3-7

4. Remote Interfaces

4.1 Network Configuration . . . . . . . . . . . . . . . . . . . . . . . 4-1

4.1.1 Network PC Access . . . . . . . . . . . . . . . . . . . . . 4-2

4.1.2 Network Printing . . . . . . . . . . . . . . . . . . . . . . 4-3

4.1.3 Automatically Print Report at End of Run . . 4-4

4.2 Direct Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4

4.2.1 Windows 2000 Settings . . . . . . . . . . . . . . . . . . 4-5

4.2.2 Windows XP Settings . . . . . . . . . . . . . . . . . . . 4-6

4.2.3 Windows Vista Settings . . . . . . . . . . . . . . . . . 4-8

4.2.4 Completing the Direct Connection . . . . . . . . 4-10

5. Maintenance

5.1 Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . 5-1

5.2 Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1

5.2.1 Collection Rack and Tray Cleaning . . . . . . . . 5-2

5.3 Tubing Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2

5.4 Flow Cell Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4

5.4.1 Post Separation . . . . . . . . . . . . . . . . . . . . . . . . 5-4

5.4.2 Quick Cleaning when Recommended . . . . . . . 5-5

5.4.3 Monthly Flow Cell Cleaning . . . . . . . . . . . . . . 5-9

5.5 Electrical Troubleshooting . . . . . . . . . . . . . . . . . . . 5-10

1-1

CombiFlash® R

Installation Guide

Section 1 Introduction

1.1 Documentation Overview

This Installation Guide provides:

• Safety Information

• Unpacking instructions

• Installation instructions, including placing the instrument on a network and direct connections with a Windows computer

• Certification and warranty information.

Once you are operating the CombiFlash R

, you may refer to the Help menu for operating instructions and further assistance.

The CD that accompanies this installation guide contains this guide in Adobe Acrobat PDF format and the PeakTrak

On-line Help in PDF format.

1.2 Product Overview

The Teledyne Isco CombiFlash Rf flash chromatography system gives you high-productivity automation, programmable gradients, full-spectrum UV detection and peak separation, and automatic detection of columns and collection tube racks. Its small size makes it a great “personal system” and well suited for operation within chemical hoods and other limited spaces.

WARNING

Avoid hazardous practices! If you use this instrument in any way not specified in this manual, the protection provided by the instrument may be impaired; this may increase your risk of injury.

CombiFlash® Rf Installation Guide

1-2

Figure 1-1 CombiFlash Rf

Control of the system is through a simple to use interface. This interface can be accessed through the touch screen panel, or a Windows computer via a direct or network Ethernet connection. These options give you the flexibility to operate and monitor the CombiFlash R

system at the instrument,

from a computer in the lab, or from remote locations.

The CombiFlash R

is optimized for use with Teledyne Isco’s

RediSep

Rf columns, which are pre-packed with a variety of

media. For example, the CombiFlash R

can purify samples

from 4 milligrams to greater than 33 grams using RediSep R

columns loaded with 4 to 330 grams of silica gel.

Applications include purification of organic compounds for drug discovery, as well as research in agrochemicals, petrochemicals, natural products, polymers, and catalysts.

Section 1 Introduction

1-3

1.3 Operating Overview

The CombiFlash Rf may be controlled through its built-in touch screen panel or by a Windows computer running Microsoft Internet Explorer 6 or newer.

The CombiFlash R

is equipped with the touch screen display for local control. For Windows computer control, the CombiFlash R

may be controlled by the computer in two different ways using TCP/IP protocol—direct or network. A direct connection uses a cross-over cable between Ethernet ports on the CombiFlash R

and computer. A network connection allows control from a computer on an established network.

Note

Teledyne Isco recommends that you obtain assistance from your Information Technology department before attempting direct or network connections to a Windows computer.

1.3.1 Multiple Control Possibilities

The system can be accessed from the built-in touch panel and up to ten network computers. The touch panel shares control with all connected computers. The system performs the most recent command from any control input.

1.3.2 File Storage

To support operation from a variety of direct and network connections, the software and all files are stored in the CombiFlash R

on an internal hard drive. This ensures that your compound purification methods and run history files can be viewed from any connection.

CombiFlash® Rf Installation Guide

1-4

1.4 Specifications

Table 1-1 Specifications

Overall Dimensions Height: 61 cm (24")

Width: 36 cm (14.1")

Depth: 43 cm (17")

Weight 24.5 kg (54 lbs)

Power Options

Input voltage range from 100 to 240 VAC, 2.0 Amps maximum

Line Frequency 50/60 Hz

Ambient Temperature 20 to 40°C (maximum temperature must be

at least 15°C below the boiling point of the solvent)

Humidity (when connected to power)

95% relative humidity maximum at 20 to 40°C

Flow Rate Range 5 to 100 ml/min

Flow Rate Accuracy ±5%

Pressure Limit Up to 200 psi (column dependant)

For columns undetected by RFID, the maximum pressure is limited to 50 psi.

Pressure Accuracy 5% of full scale

Peak Detection Modes Slope or threshold

UV Spectrum 200 to 360 nm

Wavelength Accuracy ±5 nm

Flow Cell Pathlength 0.1 mm, ±25%

Fraction Accuracy ±[2ml + (flow rate ÷ 60)]

Pollution Degree 2

Electrical Safety per EN 61010-1

Installation Category II

Maximum Altitude 2000 meters

Note 1. All specifications are preliminary and subject to change.

Section 1 Introduction

1-5

1.5 Controls, Indicators, and Features

Figures 1-2 through 1-4 illustrate the controls on the CombiFlash R

Figure 1-2 CombiFlash R

Features (Front)

1. Touch Panel LCD display – Large 10.5 inch display for system monitoring and control.

2. USB Port – Convenient, front panel port that accepts USB Flash memory drive. A Flash memory drive may be inserted into this port for transferring files, importing and exporting methods, and system software updates.

3. Adjustable Column Mount – The injection valve assembly and upper column mount slide along this mount so the system can accept a variety of column sizes.

4. On/Standby Switch – 1 = On, 0 = standby.

5. Fraction Collector Arm and Drop Former – The arm and drop former move to deposit liquid in the collection tubes.

CombiFlash® Rf Installation Guide

1-6

6. Racks and Collection Tubes – The racks hold the fraction collection tubes. Racks include an RFID tag which the system uses to read the rack type and collection tube size.

7. Sample Injection Port – Luer-type fitting to accept the sample though either a solid load sample cartridge (shown) or a liquid injection using a syringe or similar device.

8. Injection Valve – This six-way valve is automatically positioned by the CombiFlash R

according to its current mode of operation. Modes include column equilibration, sample injection, elution, column flushing, valve cleaning, and system purging.

9. Upper Column Mount – Secures the column inlet.

10.Lower Column Mount – Secures the column outlet.

11.Top Shelf – Allows storage of accessories and solvent bottles.

12.Column Expansion Ports – These ports allow the system to add column channels with an optional module. This option is not available at the time of printing.

13.Upper Drain Tube – Liquids spilled on the top shelf are carried away through this tube to a user-supplied container.

14.Ethernet Port – An 8P8C jack for a network connection using a standard CAT5 cable, or for a direct connection to a computer using a cross-over cable.

15.RS-232 Port – Serial communication port to interface with expansion modules.

16.USB Port – For control of peripheral equipment. This rear panel port is primarily for service-related functions.

17.Cooling Fan – Cools the internal electronic assemblies.

18.Check Valves – Externally-mounted pump check valves to simplify pump maintenance.

19.Solvent Level Sensing Outlet Ports – uses air or user-supplied gas to measure the hydrostatic pressure of the solvent above the weighted tubing outlet.

20.Solvent Inlet Ports – Accepts two A solvents and two B solvents.

Section 1 Introduction

1-7

Figure 1-3 CombiFlash Rf Features (Side)

Figure 1-4 CombiFlash R

Features (Back)

CombiFlash® Rf Installation Guide

1-8

21.Optional External Gas Port – An inlet for an internal pump which supplies pressurized air or user-supplied gas for solvent level sensing, waste container full detection, and system/column purges. The external gas should be regulated to 2–5 psig before connecting the source to this port.

22.Mains Power – Connects the system to AC line voltage.

23.Was te Po rts – From left to right:

• Waste Level S ense – The system uses air or user-supplied gas to measure the hydrostatic pressure of the waste above the level sense line end. The system will suspend operation when this level is too high.

• Diverter Valve Waste – The diverter valve on the fraction collector arm sends fluid to this waste port.

• Inject Valve Waste – The injection valve is cleaned after each run. The system directs fluids from this automatic cleaning routine to this port.

24.Lower Drain Tube – This tube carries away liquids spilled onto the rack area.

1.6 Safety

Before installing, operating, or maintaining this equipment, it is imperative that all hazards and preventive measures are fully understood. While specific hazards may vary according to location and application, take heed in the following general warnings:

WARNING

Liquids associated with this instrument may be classified as carcinogenic, biohazard, flammable, or radioactive. Should these liquids be used, it is highly recommended that this application be accomplished in an isolated environment designed for these types of materials in accordance with federal, state, and local regulatory laws, and in compliance with your company’s chemical/hygiene plan in the event of a spill.

Section 1 Introduction

1-9

WARNING

Avoid hazardous practices! If you use this instrument in any way not specified in this manual, the protection provided by the instrument may be impaired.

WARNING

If you are using flammable solvents or chemicals with this system, vapor concentration levels may exceed the maximum exposure levels as recommended by OSHA Guide 1910.1000. To reduce those levels to a safe exposure, Teledyne Isco recommends that you place the system in a laboratory hood designed for the purpose of ventilation. This hood should be constructed and operated in accordance with federal state and local regulations. In the event of a solvent or chemical spill, your organization should have a plan to deal with these mishaps. In all cases, use good laboratory practices and standard safety procedures.

1.6.1 Hazard Severity Levels

This manual applies Hazard Severity Levels to the safety alerts. These three levels are described in the sample alerts below.

CAUTION

Cautions identify a potential hazard, which if not avoided, may result in minor or moderate injury. This category can also warn you of unsafe practices, or conditions that may cause property damage.

WARNING

Warnings identify a potentially hazardous condition, which if not avoided, could result in death or serious injury.

DANGER

DANGER – limited to the most extreme situations to identify an imminent hazard, which if not avoided, will result in death or serious injury.

CombiFlash® Rf Installation Guide

1-10

1.6.2 Hazard Symbols

The equipment and this manual use symbols used to warn of hazards. The symbols are explained in Table 1-2.

Table 1-2 Haza rd Symb ol s

Warnings and Cautions

The exclamation point within the triangle is a warning sign alerting you of important instructions in the instrument’s technical reference manual.

The lightning flash and arrowhead within the triangle is a warning sign alerting you of “dangerous voltage” inside the product.

The pinch point symbol warns you that your fingers or hands will be seriously injured if you place them between the moving parts of the mechanism near these symbols.

Symboles de sécurité

Ce symbole signale l’existence d’instructions importantes relatives au produit dans ce manuel.

Ce symbole signale la présence d’un danger d’électrocution.

Risque de pincement. Ces symboles vous avertit que les mains ou les doigts seront blessés sérieusement si vous les mettez entre les éléments en mouvement du mécanisme près de ces symboles

Warnungen und Vorsichtshinweise

Das Ausrufezeichen in Dreieck ist ein Warnzeichen, das Sie darauf aufmerksam macht, daß wichtige Anleitungen zu diesem Handbuch gehören.

Der gepfeilte Blitz im Dreieck ist ein Warnzeichen, das Sei vor “gefährlichen Spannungen” im Inneren des Produkts warnt.

Section 1 Introduction

1-11

1.7 For Additional Information

Technical assistance for the CombiFlash Rf can be obtained from:

Teledyne Isco, Inc.

4700 Superior St. Lincoln NE 68504

Phone: (800) 228-4373 or (402) 464-0231 Fax: (402) 465-3001 E-mail: IscoService@teledyne.com

Vorsicht Quetschgefahr! Dieses Symbol warnt vor einer unmittelbar drohenden Verletzungsgefahr für Finger und Hände, wenn diese zwischen die beweglichen Teile des gekennzeichneten Gerätes geraten.

Advertencias y Precauciones

Esta señal le advierte sobre la importancia de las instrucciones del manual que acompañan a este producto.

Esta señal alerta sobre la presencia de alto voltaje en el interior del producto.

Punto del machacamiento. Sus dedos o manos seriusly serán dañados si usted los coloca entre las piezas móviles cerca de estos símbolos.

Table 1-2 Hazard Symbols (Continued)

2-1

CombiFlash® R

Installation Guide

Section 2 System Preparation

This section provides instructions for unpacking and installing the CombiFlash R

system. To prepare the system for operation, sequentially follow all instructions in sections 2.1 through 2.12.

2.1 Unpacking the Unit

The CombiFlash Rf is shipped in a single carton. Carefully unpack the shipment and inspect the contents. If there is any damage to the shipping carton or any components, contact the shipping agent and Teledyne Isco (or its authorized representative) immediately.

WARNING

If there is any evidence that the system has been damaged in shipping, do not plug it into AC power. Contact Teledyne Isco or its authorized representative for advice.

Compare the contents of the boxes with the enclosed packing slip. If there are any shortages, contact Teledyne Isco immediately.

2.2 Instrument Location

The CombiFlash Rf has a relatively small footprint, requiring about 1550 square centimeters (240 in

) of level bench space.

Ensure that the CombiFlash R

has at least 3 cm (1.25") of air space behind it for ventilation. Additional space may be required for solvent and waste containers.

Refer to Table 1-1 for environmental conditions and power requirements.

CombiFlash® Rf Installation Guide

2-2

WARNING

The system is heavy. Use a two-person lift to prevent injury.

Before making any connections to the CombiFlash Rf, place the system on the bench or in the fume hood where it will be operated. Temporarily position the system so you can access the back panel to complete the connections.

2.3 Connect Power

Ensure that the On/Standby switch below the touch screen panel is in the Standby position. Then, use the supplied IEC power cord to connect the CombiFlash R

to mains power.

WARNING

Mains power must meet the voltage, frequency, and amperage requirements listed on the serial number label.

2.4 Connect Solvent Lines

WARNING

Risk of fire ignited by electrostatic discharges. Never substitute the black tubing on CombiFlash systems. The black PTFE tubing (P/N 023-0503-06) is conductive. This tubing is required to dissipate static electricity.

CAUTION

To prevent damage or premature wear to the pump and internal valves, clean solvent should be used. The solvent should not contain any dissolved solids.

The CombiFlash Rf has four solvent inlet ports on the back panel: two A solvents and two B solvents. The system requires at least one A and one B solvent to form a binary gradient, and assumes that the B solvent is stronger than A. The second set of inputs allow you to form alternative binary gradients, or change the A or B solvent mid-run.

Accessory package (P/N 60-5239-006) includes several pieces to complete the solvent inlet connections.

Section 2 System Preparation

2-3

Figures 2-1 and 2-2 show the recommended connections when the user-supplied solvent container has a 38 or 45 mm opening (GL 38 or GL 45). Note that there are two different styles that can ship with the system. One styles includes a metal plate and larger opening on the cap (Figure 2-1), the other has no plate and a smaller opening on the cap (Figure 2-2).

Figure 2-1 Recommended solvent connection, with plate

60-0923-017 Ferrule

60-0923-015 Compression Fitting Nut

60-5234-130 Label (1 of 4)

60-5235-042 38 mm Cap, or 291-0010-06 45 mm Cap

60-5233-399 38 mm Plate, or 60-5233-400 45 mm Plate

60-5234-129 Inlet Filter Assembly (Place weighted filter at bottom of container.)

To Solvent Level SensingTo Solvent Supply

Connection

CombiFlash® Rf Installation Guide

2-4

Figure 2-2 Recommended solvent connection, without plate

If the container does not have a GL 38 or GL 45 opening, omit the use of the cap and plate. Ensure that the solvent and air tubing are secured so that the weighted filter remains at the bottom of the solvent source.

60-0923-017 Ferrule

60-0923-015 Compression Fitting Nut

60-5234-130 Label (1 of 4)

60-5235-050 38 mm Cap, or 60-5235-051 45 mm Cap

60-5234-129 Inlet Filter Assembly (Place weighted filter at bottom of container.)

To Solvent Level SensingTo Solvent Supply

Connection

Section 2 System Preparation

2-5

The Solvent Level Sensing air line connects to the back panel with a compression fitting. This fitting must be airtight. To connect tubing using the compression fittings:

1. Slide the nut and ferrule onto the tubing as shown in Figure 2-1 or 2-2.

2. Fully insert the tubing into the threaded bulkhead fitting on the back panel of the system.

3. Finger-tighten the nut onto the threaded bulkhead fitting. This will seat the ferrule in the fitting.

Note

When using higher-density solvents such as dichloromethane (DCM), place the solvent container level with or above the CombiFlash Rf system. Placing solvent containers below the level of the Rf can contribute to decreased flow due to the high vapor pressure of DCM. This problem becomes more pronounced as the ambient temperature increases.

2.5 Connect Waste Lines

WARNING

Risk of fire or equipment damage. Failure to connect Waste Port tubing may allow organic solvents to pool in unsafe areas, possibly creating dangerous levels of flammable vapors.

WARNING

CAUTION

Elevated flammable vapor levels are possible. Ensure that the waste container is adequately ventilated, preferably by placing it in a fume hood.

The system has two waste outlets on the back panel: Diverter Valve waste and Inject Valve waste. You can route waste to a common collection container, or to individual containers.

CombiFlash® Rf Installation Guide

2-6

The Waste Level Sense uses air pressure to detect the liquid level in the common waste container. If using individual containers, use the waste level sense to detect the level of the Diverter Valve waste container. Under normal operating conditions it will fill faster than the Inject Valve waste container. Empty both containers at the same time to prevent overfilling the unmonitored container.

Accessory package (P/N 60-5239-006) includes parts to complete the waste connections. Figure 2-3 shows the recommended connections for user-supplied waste containers with either a 38 or 45 mm opening (GL 38 or GL 45). Note that there are two different styles that can ship with the system. One styles includes a metal plate (Figure 2-3), the other has a plastic plate with four small openings on the cap (Figure 2-4).

Refer to the steps in section 2.4 to connect the tubing to the system using the compression fittings. Then, complete the connections according to Figure 2-3 or 2-4.

If your connection hardware matches Figure 2-3, connect the Waste Level Sense line to the compression fitting in the center of the cap. Push the ends of the two black waste lines through the holes in the cap.

If your connection hardware matches Figure 2-4, push the three tubes through the cap. Push the stop on the Waste Level Sense tubing against the cap. This ensures that the Waste Level Sense tubing is far enough into the container to detect when it is nearly full.

Should the container not have a GL 38 or GL 45 opening, omit the use of the waste cap. Ensure the solvent tubes are secured so they drain into the waste container. Secure the Waste Level Sense air tubing so its outlet is at least two inches (5 cm) below the container’s maximum level.

Note

When using higher-density solvents such as dichloromethane (DCM), ensure that the waste container is no more than 3 feet below the supply solvent levels. Placing solvent containers above the system and waste containers on the floor may cause the internal check valves to open and allow solvent to flow through the system when in the standby state.

Section 2 System Preparation

2-7

Figure 2-3 Recommended waste connections, with metal plate

60-0923-017 Ferrule

60-0923-015 Compression Fitting Nut

60-5234-143

Waste Tubing Assembly

60-5234-051 38 mm Waste Cap, or 60-5234-142 45 mm Waste Cap

To Diverter Valve Waste Connection

To Waste Level

Sense Connection

To Inject Valve Waste Connection

CombiFlash® Rf Installation Guide

2-8

Figure 2-4 Recommended waste connections, with plastic plate

60-0923-017 Ferrule

60-0923-015 Compression Fitting Nut

60-5234-143

Waste Tubing Assembly

60-5235-053 38 mm Waste Cap, or 60-5235-054 45 mm Waste Cap

To Diverter Valve Waste Connection

To Waste Level

Sense Connection

To Inject Valve Waste Connection

Tubing Stop

Ventilation Hole (Luer fitting) If necessary, connect user-supplied tubing and route to fume hood.

Section 2 System Preparation

2-9

2.6 Optional External Gas

The CombiFlash Rf system has an internal air pump that provides compressed air for solvent and waste level sensing. Optionally, the system can deliver a compressed gas. Inert or other gases may be more suitable than air for some applications.

If ambient air is compatible with your solvents and waste, simply leave the Optional External Gas port open.

If you want to use a gas instead of air, connect user-supplied

/8" I.D. tubing to the Optional External Gas port. Connect the

other end to the user-supplied compressed gas. The external compressed gas should be dry, filtered, and regulated to 2– 5 psi (0.14–0.34 atm, 13.8 –34.5 KPa).

2.7 Connect and Route Drain Lines

WARNING

Risk of fire or equipment damage. Failure to connect drain lines may allow organic solvents to pool in unsafe areas, creating a potential for dangerous levels of flammable vapors. Improper draining may damage the instrument’s internal components.

The CombiFlash Rf has drain tubes extending from its top shelf and back panel. The tubes drain away any liquid spilled on the top shelf and the tray beneath the fraction collection racks. Route the end of this tubing to a suitable waste fluid collection container.

Note

It may be necessary to extend the drain tube. If so, splice the tubing with user-supplied tubing. The user-supplied tubing should have an inside diameter no smaller than the existing drain tubing, and must be compatible with the solvents used by the system. Route this extension tubing to the waste collection vessel.

2.8 Position the System

After completing the various connections, the system can be moved to its operating position. Turn the system so that the operator can access all of the front view features and controls (Figure 1-2). Use care not to damage the connections, tubing, and cables while moving the system.

CombiFlash® Rf Installation Guide

2-10

2.9 Install Collection Tube Racks

Before beginning a run, you must load collection racks with tubes onto the system’s fraction collector tray.

Your system was shipped with two collection tube racks. The following tube rack sets are available:

• 60-5237-031 – Two racks for 16×125 mm test tubes (15.5 mL). Total tubes: 150.

• 60-5237-032 – Two racks for 16×150/160 mm test tubes (18 mL). Total tubes: 150.

• 60-5237-033 – Two racks for 18×150 mm test tubes (25 mL). Total tubes: 140.

• 60-5237-034 – Two racks for 18×180 mm test tubes (30 mL). Total tubes: 140.

• 60-5237-035 – Two racks for 25×150 mm vials (50 mL). Total vials: 60.

• 60-5237-040 – One rack for 500 mL French square bottles.

To load the racks:

1. Insert test tubes, vials, or bottles into the rack (Fig. 2-5).

CAUTION

Risk of broken glass or equipment damage. Do not load test tubes longer than the length listed on the tube size label.

2. While holding the rack with the tube size label visible (Figure 2-6), insert the racks into the system. Slide the rack in until you feel it drop into its seated position.

CAUTION

An incorrectly installed rack will cause the rack to be misaligned under the fraction collector arm. Misaligned racks might cause fractions to miss the tube opening or deposit in the wrong tube. Always ensure the tube size label is visible (that is, facing outward) and the rack is pushed in until it is seated.

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2-11

When you turn the power switch to on, the system will automatically detect the type of rack, and configure program settings accordingly. Later, in section 2.11.6, you can configure the maximum volume for each tube size.

Figure 2-5 Loading test tubes

Figure 2-6 Inserting the collection tube rack

Tube Size Label

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2.10 Turn on Power

The system’s power switch is located just below the touch screen panel. Turn the switch to the ON position. The system will begin its startup routine which includes self diagnostics. The system is ready for operation when the PeakTrak screen is displayed.

2.11 Configure the System

Before operating the system, it should be configured for the desired operation. To configure the system, open the Configuration window by selecting Tools>Configuration from the PeakTrak menu.

The configuration window has two tabs: Instrument Configuration and Network Configuration. Adjust the following (sections 2.11.1 through 2.11.9) on the Instrument Configuration tab for the desired operation and then click OK to save the settings. Network Configuration settings are discussed later in Section 4, Remote Interfaces.

2.11.1 Solvents

When you installed the system, up to four solvents were connected to the back panel. This section of the Configuration window allows you to manage these solvents. To do so:

Note

The system is shipped with common solvent names already loaded. If your solvent names are listed in the solvent drop-down list boxes, skip steps 1 through 3.

1. Click the “Add Solvent” button.

2. Enter the solvent name and click the OK button.

3. Repeat steps 1 and 2 for all four solvents.

4. For the Solvent A1 drop-down list box, select the solvent name connected to the A1 Solvent Inlet Port. Repeat for Solvents A2, B1, and B2.

5. Select the “Enable solvent level sensing” check box to enable this feature (recommended). Clear this box to disable this feature.

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The solvent level sensing feature will monitor solvent usage to minimize the risk of running out of solvent during a purification run. The system compares the volume required for a purification run with the estimated volume in the solvent container and alerts you when there is not enough.

6. If using the solvent level sensing feature, enter the Minimum Solvent Level (density dependent) as a range in centimeters.

To understand this range, consider that dichloromethane is more dense than hexane. If the selected range is 2–4, the system triggers an alert when the dichloromethane level falls to about 2 cm above the weighted filter. At the same selected range, the system would trigger an alert when the hexane falls to about 4 cm above the weighted filter.

2.11.2 General Settings

CombiFlash Rf Name (optional) – Use this option to name your system. The name will appear in operational displays and run summaries. This feature is useful when your laboratory has more than one CombiFlash R

system.

Language – Select the desired language from the drop-down list box.

2.11.3 Vapor Limit

The system has an internal vapor sensor that detects vapors present in the immediate atmosphere. When the limit is exceeded, the CombiFlash R

will shut down to avoid a

hazardous condition.

Teledyne Isco recommends using the default setting of 25. This value represents an organic vapor level slightly above the ambient vapor level of a well-ventilated laboratory.

A setting below 25 could cause random alarms without significant vapors present. If PeakTrak displays a Vapor Limit alarm while the Vapor Limit is set at 25, perform the following checks on your laboratory and the instrument:

• Ensure that no open containers or spills of organic solvent are in close proximity to the system.

• Ensure that the system is located in a well-ventilated area.

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• Ensure that there is no visible solvent leakage from the system.

If PeakTrak continues to display the Vapor Limit alarm after you have made these checks and corrected any problems found, it is likely that organic vapors are present in the ambient environment of your laboratory. In this case, increase the setting of the Vapor Limit. Settings greater than 25 are appropriate for laboratory environments with a somewhat elevated background solvent vapor concentration, representing a safe setting, but one with a reduced margin for error.

2.11.4 Automatically Print Report at End of Run

If this option is enabled, the system will print a report at the end of each run.

Note

This option requires the system to configured for network operation and a connection to a printer on the network. Network settings are discussed in Section 4, Remote Interfaces. Do not select this option for these initial installation steps.

2.11.5 Enable Run Length Extension

When enabled, this option automatically extends the run if a peak is eluting at the end of the maximum %B gradient. This ensures that a late-eluting peak fully comes off the column and is collected.

An automatic run extension is a five-minute isocratic hold added to the end of the run’s maximum %B gradient profile. During the extension, the system continues to pump the maximum %B solvent mixture. Should the system still detect a peak after an extension, the system will add another, up to a maximum of three extensions.

Occasionally, compounds might come off the column once the %B returns to the minimum value at the end of a run. If the Run Length Extension is enabled, it will automatically extend the run one time to clear the column and plumbing of any remaining material.

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Figure 2-7 Automatic Run Extension Examples

Figure 2-7 illustrates the possible run extensions. The original method was programmed to rise to the maximum %B over seven minutes, hold for two minutes and return to the minimum %B for a final minute. At nine minutes, a peak was eluting. The system extended the run, holding the %B at the maximum level for another five minutes. This also occurred at fourteen and nineteen minutes, resulting in the second and third extensions. At 24 minutes, the %B solvent strength returned to zero. Before the final minute elapsed, more compound was detected, causing the system to extend the run for a final five minutes at the minimum %B.

2.11.6 Set Default Tube Volumes

Click this button to open a window from which you can set the default volume of the collection tubes. You can increase or decrease these values to set the desired default volume collected in each container. Just be sure you don’t overflow the containers by exceeding their capacity.

The system will automatically advance to the next tube when this default volume is met in each tube. Keep in mind that advanced method settings (discussed in Section 3 and the on-line help) may override this default setting. During a run, other factors such as automatic tube advances for detected peaks will affect collected volume.

2.11.7 Set Date/Time

Click this button to open a window from which you can set the system date and time.

0 5 10 15 20 25

Original method

Extension 1

Extension 2

Extension 3

Final Extension

Minutes

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To prevent unauthorized time changes, this feature is password protected. The system is shipped with the password set to combiflash. Use the Tools>Set Password menu command to change this password for greater security.

2.11.8 Default Run Units

Run units are displayed along the X-axis of the chromatogram. Select Time (in minutes) or Column Volumes. A column volume unit is the time it takes to pump enough solvent to exchange the volume held by the column. The duration in minutes will vary according to the column media and size, and the flow rate.

2.11.9 Gradient Method

Select the standard gradient type (Figure 2-8).

• Linear – The system gradually mixes solvents A and B from the last programmed %B until it reaches the next programmed %B. This method connects the inflection points that define the gradient with a straight line.

• Step – The system holds each %B value until it reaches the next programmed %B. Because the system holds the %B values, the changes at each new value are nearly instantaneous, producing a stepped appearance on the plot area.

• Isocratic – The system holds the initial solvent mix for the entire run.

Figure 2-8 Gradient types

IsocraticStepLinear

Section 2 System Preparation

2-17

2.12 Prime the Solvent Lines

Before the first use, the system should be primed. Ensure that the solvent containers are filled, then:

1. Select the “Tools>Auto prime” menu command.

2. Select the desired A and B solvents from the drop-down list boxes.

3. Click the Play button to start priming the system.

The system pumps 100% Solvent B through the system and out the Waste port, and then repeats with 100 % Solvent A. (This B-A order leaves the internal lines filled with solvent more appropriate for the beginning of a purification run.)

Note

When priming the first time, inspect the solvent and waste connections to the system. If any leaks are observed, click the Cancel button to stop the Auto Prime. Correct the leak by tightening the fitting an additional

/4 turn, and then restart the Auto

Prime from step 1.

To advance to the next Auto Prime step, you can click the Fast Forward button. The Auto Prime window closes when finished.

After Auto Priming, the system is ready for operation (Section 3).

Note

Use Auto Prime for quick solvent changes by pumping a fixed amount of solvent through the waste fluid path at 100 mL/min. For more advanced priming functions such as varying the flow rates, fluid paths, etc., or to purge the system with air before changing between normal and reversed phase solvent systems, use the Tools>Manual Control option.

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CombiFlash® R

Installation Guide

Section 3 Operation

This section provides abbreviated operating instructions for the CombiFlash R

. For complete instructions, refer to Help

menu option from PeakTrak’s main menu.

3.1 Sample Preparation

Before starting a run, consider how the sample will be introduced to the column media. This section discusses three methods: liquid injection, solid sample cartridges, and preloading the sample on the column.

3.1.1 Liquid Sample Injection

If the sample is soluble in the starting mobile phase, it can be prepared as a solution and injected onto the column when prompted during the purification run.

3.1.2 Solid Samples

Some compounds are not soluble in solvents that are compatible with the chromatography. In addition, the compounds may have very limited solubility in any solvent, resulting in sample volumes that are impractical for good chromatography. The solution in this case is solid sample introduction. Here the reaction mixture or dissolved sample is mixed with the same media in the chromatography column.

Some samples of this type may be simply dissolved and placed into a prefilled cartridge. You can then use the cartridge immediately, or dry it by vacuum before placing it on the system.

Other samples may need more care. Typically you would create a mixture of 20% sample load to media (w/w). Then dry the mixture under conditions that will drive off the solvent without affecting the compounds of interest. These compounds

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remain bound to the media. Once dried, pour the media/sample mixture into an empty cartridge.

To prepare an empty solid sample cartridge:

1. Ensure the empty cartridge has a bottom frit.

CAUTION

Missing frits may cause equipment damage, UV detection problems, or increased maintenance. Frits prevent solids from entering the fluid path.

2. Prepare the media and sample:

a. Dissolve your sample in a minimal amount of a suitable,

volatile solvent.

b. Place the media into the solvent. If using silica gel, a

particle size of 40–60 µm (240–400 mesh) is recommended. The amount of silica required is about four to five times the mass of your sample.

c. Agitate the solvent for a moment to allow the sample to

adsorb to the silica.

d. Remove the solvent with a suitable method, such as

rotary evaporation.

3. Load the media and sample mixture into the cartridge. Tap the cartridge on the benchtop to settle the mixture.

4. Place a frit on the top of the cartridge. Force the frit down against the mixture using the plastic plunger.

5. Wipe any residual powder inside the neck of the cartridge.

Empty solid sample cartridges also allow a variety of adsorbents, such as diatomaceous earth, boiling chips, cotton balls, or paper wipes. Even with alternative adsorbents, always use top and bottom frits to prevent fluid path problems.

After you have prepared the pre-filled or empty cartridge, place the solid sample cartridge on the system:

1. Attach the desired adjustable cartridge cap to the system.

2. Align the cap and cartridge and push them together.

3. Rotate the cartridge

/4 turn so that the cap will hold the

cartridge.

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3-3

4. Press the tab on the cap and push the plunger into the cartridge until it rests against the top frit.

5. Release the tab on the cap. Note that the opposite end of the tab secures the cartridge.

6. Load the solid sample cartridge with cap on the sample injection port.

3.1.3 Preloading on Column

You can load the reaction mixture or sample directly onto the column, sometimes called “direct” or “dry” loading.

Note

If using this method, use care to ensure that a column equilibration does not wash away the sample. Bypass the column equilibration at run time by selecting “Preload on column” as the sample Loading Type. Refer to Section 3.3 for more details.

3.2 Loading a RediSep Rf Column

To loa d a RediSep Rf column:

Note

For best results, always use RediSep Rf columns. The system will not automatically detect other columns, including non-Rf RediSep columns. The system also limits the maximum operating pressure to 50 psi when the column is not detected.

1. Select a RediSep Rf column. The on-line help includes a column selection guide that can assist you in selecting a

stationary phase media and column size.

2. Raise the injection valve and insert the column into the top column fitting. Note that the column fittings are keyed to ensure the correct flow direction.

3. Slowly lower the injection valve while aligning the bottom column fitting. The spring-loaded injection valve will hold the column in place.

4. To seal the column fittings, give the column a slight twist (

/4 turn).

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Note

After loading a RediSep Rf column, the system will use RFID technology to automatically detect the media type and column size. PeakTrak displays the detected column size on the Main and Method Editor windows. If the system does not detect the column, manually select the column media and size.

3.3 Start a Default Method

After completing the installation steps in Section 2, preparing the sample, and inserting the column, you are ready to perform a run with the default method. The system’s default methods are factory-set with run parameters typically used by chemists. Default methods are optimized for the use of RediSep R

columns. The default settings will:

• equilibrate the column

• collect all fluid in the fraction collector rack

• differentiate between UV vs. non-UV absorbing fluid and place the fluids into separate tubes

• cut UV absorbing peaks based on slope detection or level threshold.

To start the run from the PeakTrak Main window:

1. Enter a sample name. If you choose not to, PeakTrak will enter the date and time as the sample name when you start the run.

2. Review the PeakTrak Main window settings. If you want to change any settings, refer to the Editing a Method on-line help topic.

3. Click the Play button.

4. Select the sample Loading Type from the list. This Loading Type should support the sample preparation you chose in Section 3.1. Possible sample loading types are:

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3-5

• Cartridge w/ (with) pause – Select this option if you intend place the sample into a solid sample load cartridge, but have not yet prepared the sample. When you click the run button, the system will perform a column equilibration and then wait while you prepare the cartridge. After you have placed the cartridge on the system, click OK to continue with the run.

• Cartridge w/o (without) pause – Select this option if you have prepared the sample and placed it into a solid sample load cartridge. The system will proceed automatically until the end of the programmed run length.

• Liquid Inject – Select this option if you have prepared a liquid sample and plan to manually inject it into the injection port after column equilibration.

• Preload on column – Select this option if you have preloaded the sample on the column. The system will skip column equilibration so that the sample will not be flushed from the column before the run.

5. Review or update the Start Rack and Start Tube.

6. Review the Minimum Run Requirements. The system will report the estimated solvent volumes, expected waste, collection tube usage, etc. You can use this information to verify that there will be enough solvent to complete the run, the waste volume does not exceed the collection container’s capacity, and whether or not more tubes will be required during the run.

Note

The system estimates the solvent volumes by monitoring the solvent level in the container and the known usage rate. The system continues to refine this estimate during operation.

Note

If the waste level sensing tube is inserted correctly into the waste container, the system automatically will suspend operation before an overflow condition might exist. To prevent the run from being suspended before completing the run, ensure that the container will hold the expected waste volume.

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7. Click OK and the run begins. The system responds according to the sample Loading Type you selected in step 4.

If you selected Cartridge w/ pause, the system equilibrates the column with the starting %B and then waits while you prepare the solid sample load cartridge. Place the cartridge on the system and click OK to continue.

If you selected Cartridge w/o pause, the system equilibrates the column and immediately starts the separation.

If you selected Preload on column, the system skips the equilibration and immediately starts the separation.

If you selected Liquid, the system equilibrates the column and then waits. When instructed, perform the following steps:

a. Place the injection syringe on the injection port.

b. Slowly force the liquid into the injection port.

c. Chase the first injection with a second injection solution

of at least 0.25 mL. The chase solution can be the starting mobile phase or diluted sample mixture.

d. Click OK to continue the run.

3.4 During the Run

You may allow system to proceed with the run while monitoring the progress on the PeakTrak main window. If desired, gradient parameters may be modified during the run. (See the Real-time Gradient Editing on-line help topic.)

As the run progresses, the absorbance trace is drawn on the Gradient Plot area. The separation or purification continues until the end of the run defined by the run length setting.

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3-7

3.4.1 Run Control Buttons

You clicked the Play button to start the run. During the run, other run control buttons are active.

• Pause — The Pause button holds the %B at the current value while the system continues to operate (sometimes called an isocratic hold). Note that pausing the run extends the run length. While in the Paused state, you can resume the run by clicking the Play button, or stop the run by clicking the Stop button. If you resume the run, the system continues with the gradient curve at the %B when the system was paused.

• Stop — This button suspends the entire run. Unlike the Paused state, the pump, peak detection, and fraction collection will not operate. While stopped, you can save the run data by selecting the File>Save Run as PDF or Save Run as Text from the menu, end the run by clicking the Rewind button, or resume the run by clicking the Play button.

• Next Tube — This button advances the fraction collector to the next tube position. This allows you to conveniently collect elute of interest in a new tube.

Note

When you click the Next Tube button, the system immediately marks the tube advance on the chromatogram. However, the system delays the movement of the drop former over the tubes. This delay accounts for the volume held in the tubing between the detector and the drop former, sometimes called the “delay volume.” It is important to remember that the chromatogram displays activity in real time while the fraction collector activity lags behind. The duration of this delay will vary with the flow rate.

• Rewind — This button is active when the system has completed the run, or if the run was stopped by clicking the Stop button. The Rewind button returns you to the Main window with the current method.

If you have stopped the run before its programmed run length has elapsed, clicking the Rewind button changes the current method to the new, shorter run length. This modified method is ready for the next run, or can be saved for future runs.

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• Fast Fo rwar d — Click this button to jump to the next step of a run.

Once you have started a run, the system performs several steps. The first step is to deliver solvents using the programmed gradient for the entire run length. When this step is complete, the system will purge the column with air and clean the injection valve. Clicking the Fast Forward button will cause the system to skip any remaining time in the current step and advance to the beginning of the next step. Unlike the Rewind button, the clicking the Fast Forward button to complete the run will not modify the current method’s run length setting.

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CombiFlash® R

Installation Guide

Section 4 Remote Interfaces

This section provides instructions for controlling the CombiFlash R

system through a remote interface. The system can be accessed by several personal computers through a corporate network, or by a single personal computer (PC) through a direct connection.

4.1 Network Configuration

Note

The procedures described in this section will require assistance from your network administrator. Contact your Information Technology department before proceeding.

The system has a factory-assigned IP address— 192.168.1.51. In many cases, this address must be reconfigured for use on a corporate network. To reconfigure the IP address:

1. From the touch screen panel, select the Tools>Configuration menu command.

2. The Configuration window has two tabs. Select the Network Configuration tab.

3. Select the Network Type. The options are “Static IP” and “DHCP”.

Static IP – If you select “Static IP,” configure the IP Address, Netmask, and Gateway with the information provided by your network administrator.

DHCP – Before considering DHCP, review the three following questions with your network administrator. If you can answer Yes to all questions, then DHCP is an option for your system.

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• Is it possible to assign a static IP address based on the MAC address of the instrument? (Administrators may

use this method to assign static addresses through the DHCP server instead of directly on the instrument, simplifying the management of static IP addresses within the organization.)

Note

A label on the system’s back panel lists its MAC Address. You also can find the MAC Address on the Help>About PeakTrak window.

• Can the DHCP server support an infinite lease for the instrument?

• Can the DHCP server automatically update the DNS records after the IP address is given to the instrument?

If you select “DHCP,” enter a unique Instrument Name. The name will be sent with the DHCP request and will be used to update the DNS settings. This name would allow you to assign an Instrument Name such as “My_Rf.” Users would then access the instrument through the address “http://My_Rf.”

4. Click the OK button to save the settings.

5. Confirm that your network administrator has completed any necessary network changes to support the system.

6. Locate the CAT5 connection cable (P/N 480-6545-01) in the accessory package. Insert one end into the Ethernet port on the back panel. Connect the other end of the cable to your network access port.

You should be able to connect to the CombiFlash R

from a PC on the network (Section 4.1.1) and set up a network printer (Section 4.1.2).

4.1.1 Network PC Access

A successfully networked CombiFlash Rf system can be accessed by a PC that meets the recommendations listed in Table 4-1.

To access the system simply open an Internet Browser and enter the correct address.

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• If the system was configured with an IP address, access the system from a network computer by entering “http://___.___.___.___”, where the blanks are replaced by the selected address.

• If the system was configured for DHCP and a network name, access the system from a network computer by entering “http://____________”, where the blank is replaced by the Instrument Name.

The browser window will load PeakTrak after you enter the address.

4.1.2 Network Printing

The CombiFlash Rf system can print to a network printer and supports both JetDirect and line printer (LPR) queues.

Consult with your network administrator to determine the IP address of selected printer. If the printer uses an LPR print queue, you must also find out the queue name. If the printer uses a JetDirect print queue, also ask for the port number. When this information is known, you can proceed with configuring system for network printing.

1. Select the Tools>Configuration menu command.

2. The Configuration window has two tabs. Select the Network Configuration tab.

3. Follow the on-screen instructions for entering the address and queue information.

Table 4-1 Personal Computer Recommendations

Operating Systems: Microsoft Windows 2000, XP, or Vista

Hardware: The computer hardware must meet the minimum

required specifications of the selected operating system.

Network Protocol: TCP/IP

Network Connection: IEEE 802.3 (Ethernet)

Display: 800 x 600 pixels, 256 colors, minimum

Internet Browser: Microsoft Internet Explorer 6.0 or later.

a. This table shows supported PC configurations. Other configurations or

AJAX-compatible browsers may be possible but are unsupported by Teledyne Isco.

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4. Click OK to save the settings. The CombiFlash Rf system will send a test page to the printer.

After successfully printing a test page, the network printer will be available for printing using the File>Print menu command or through the Automatically Print Report at End of Run feature described below.

4.1.3 Automatically Print Report at End of Run

If the CombiFlash Rf system can successfully print to a network printer (Section 4.1.2), it may be configured to print a report at the end of each run. The report includes the method settings, chromatogram, and peak/tube collection information. To enable this feature:

1. Select the Tools>Configuration menu command.

2. The Configuration window has two tabs. Select the Instrument Configuration tab.

3. Select the “Automatically Print Report at End of Run” option.

4. Click OK to save the setting.

4.2 Direct Connection

A direct connection supports communication between the CombiFlash R

system and a single PC that meets the

recommendations in Table 4-1.

This guide provides instructions for Windows 2000 (section

4.2.1), Windows XP (4.2.2), and Windows Vista (4.2.3). Refer to the applicable section, then follow the instructions in section

4.2.4 to complete the direct connection.

Note

A direct connection requires a “crossover” CAT5 cable. Standard CAT5 network cables will not work. You can purchase a crossover cable locally or ask your Information Technology department to assemble one. You can also order a crossover cable (part number 480-6545-02) from Teledyne Isco.

Note

These instructions assume that the system is using the factory-set IP address of 192.168.1.51.

Section 4 Remote Interfaces

4-5

Note

The following instructions may require a user account with Administrator privileges on the PC. If you cannot modify the settings in sections 4.2.1 through 4.2.3, contact your Information Technology department.

4.2.1 Windows 2000 Settings

1. From the Windows Start button, select “Settings>Control Panel” to view the control panels.

2. Locate the “Network and Dial-up Connections” icon and open this control panel.

3. Highlight the “Local Area Connection” icon. View the properties by right-clicking and selecting “Properties.” The Local Area Connection Properties Window will open (Figure 4-1).

4. Highlight the “Internet Protocol (TCP/IP)” item in the list, and click on the “Properties” button. The Internet Protocol Properties Window will open (Figure 4-2).

Note

The following steps change the local area connection settings. If the PC must be restored to its original network configuration, record the present Internet Protocol (TCP/IP) settings now.

5. Click the “Use the following IP address” option.

6. Enter the IP address “192.168.1.200”.

7. Enter the default Subnet Mask “255.255.255.0.”

8. Click the OK button to close the Internet Protocol properties window. Then, click the OK button to close the Local Area Connection properties window.

9. Shut down the PC and place the CombiFlash R

system in

Standby.

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Figure 4-1 Local Area Connection Properties Window

Figure 4-2 Internet Protocol Properties Window

4.2.2 Windows XP Settings

1. From the Windows Start button, open the Control Panel.

2. Locate the Network Connection icon and open this control panel.

Section 4 Remote Interfaces

4-7

3. Highlight the “LAN or High-speed Internet Connection” icon. Select the “Change settings of this connection” option, or right-click and select “Properties.” Refer to Figure 4-3.

4. Highlight the “Internet Protocol (TCP/IP)” item in the list, and click on the “Properties” button. Refer to Figure 4-4.

5. Select the Alternate Configuration tab. Click the “User Configured” option. See Figure 4-5.

6. Enter the IP address “192.168.1.200”.

Figure 4-3 LAN or High-speed Internet Connection

Figure 4-4 Local Area Connection Properties

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Figure 4-5 Alternate Configuration Settings

7. Enter the Subnet Mask, “255.255.255.0.”

8. Click the OK button to close the Internet Protocol properties window. Click the Close button to close the Local Area Connection properties window.

9. Shut down the PC and place the CombiFlash R

system in

Standby.

4.2.3 Windows Vista Settings

1. From the Windows Start menu, right-click on Network, then select the Properties menu option. The PC displays the Network and Sharing Center.

2. Under Tasks, select Manage Network Connections.

3. Right-click on the Local Area Connection icon and select the Properties option. After you provide permission to continue, the PC displays the Local Area Connection Properties window (Figure 4-6).

4. Select Internet Protocol Version 4 (TCP/IPv4), then click the Properties button. The PC displays the Internet Protocol Version 4 (TCP/IPv4) Properties window (Figure 4-7).

Section 4 Remote Interfaces

4-9

Figure 4-6 Local Area Connection Properties

Figure 4-7 Internet Protocol Version 4 (TCP/IPv4) Properties

CombiFlash® Rf Installation Guide

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Note

If the Internet Protocol Version 4 (TCP/IPv4) option is not listed, click the Install button to add it. If assistance is needed, press the F1 keyboard button to display Windows Vista Help.

Note

The following steps change the local area connection settings. If the PC must be restored to its original network configuration, record the present Internet Protocol (TCP/IP) settings now.

5. Select the “Use the following IP address” option.

6. Enter the IP address “192.168.1.200”.

7. Enter the Subnet Mask, “255.255.255.0.”

8. Click the OK button to close the Internet Protocol Version 4 (TCP/IPv4) Properties window. Click the OK button to close the Local Area Connection properties window.

9. Shut down the PC and place the CombiFlash R

system in

Standby.

4.2.4 Completing the Direct Connection

1. Connect the PC to the CombiFlash Rf system using the cross-over cable.

2. Turn the system’s On/Standby switch to ON. Wait for the PeakTrak operating screen to appear on the CombiFlash R

system, then start the PC.

3. Start Internet Explorer and type the factory default address “http://192.168.1.51”. The browser will display the PeakTrak screen.

Note

The PeakTrak screen indicates that the direct connection is working.

The CombiFlash Rf system and the PC are now configured for communication through a direct connection. Refer to PeakTrak’s on-line help for operating instructions. Abbreviated instructions can be found in Section 3 of this guide.

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CombiFlash® R

Installation Guide

Section 5 Maintenance

5.1 Preventive Maintenance

The system requires preventive maintenance for safe and reliable operation. Refer to the schedule below for the minimum periodic maintenance requirements.

As Needed – Perform these tasks as conditions require:

• Cleaning (section 5.2).

• Quick flow cell cleaning when recommended by a system alert message (section 5.4.2).

Every Run – Allow the separation run to finish with a high percentage of solvent B to flush residual compounds from the column, internal tubing, and flow cell. Refer to section 5.4.1.

Nightly – Log off the system (File> Log out) and place the

On/Standby switch in Standby.

Monthly – Perform these tasks at least monthly, more frequently if conditions warrant:

• Tubing Inspection (section 5.3).

• Collection rack and tray cleaning (section 5.2.1).

• Monthly flow cell cleaning (section 5.4.3).

5.2 Cleaning

To clean the exterior surfaces, use distilled water with a mild detergent. Use isopropyl alcohol for tougher stains.

On printed areas such as labels, avoid rubbing vigorously or using aggressive solvents like acetone. Each will ruin the printed text.

CombiFlash® Rf Installation Guide

5-2

CAUTION

Do not immerse the instrument in a water bath. The instrument is not watertight and this action could damage the internal electronics.

5.2.1 Collection Rack and Tray Cleaning

WARNING

Risk of fire or equipment damage. Unclean collection racks and tray might inhibit their conductive properties. The racks and tray must be kept clean to dissipate static electricity.

The collection tube racks and tray are made of conductive plastic. Dirt, film, or coatings might prevent their ability to dissipate static electricity. To avoid problems that possibly result from an electrostatic discharge, clean the racks and tray monthly. Use distilled water with a mild detergent. For tougher stains, use isopropyl alcohol.

5.3 Tubing Inspection

WARNING

Risk of fire or equipment damage. Faulty tubing, fittings, and drains may allow organic solvents to pool in unsafe areas, creating a potential for dangerous levels of flammable vapors. Improper draining may damage the instrument’s internal components.

Perform a tubing inspection monthly:

1. Visually inspect the solvent, waste, and drain tubing. The tubing must be free of any damage, kinks, or deterioration. Fittings should show no signs of leaks.

2. Test the collection tray drain and top shelf drain by connecting a vacuum or air supply source to the outlet end of the drain tubes. Then, verify the presence of such vacuum or air supply source on the drain hole (Figures 5-1 and 5-2).

Correct any deficiencies before returning the instrument to operation.

Section 5 Maintenance

5-3

Figure 5-1 Collector tray drain hole

Figure 5-2 Top shelf drain hole

Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the collection tray drain hole.

Vacuum or pressurized air applied to the outlet end of the drain tube must exist at the top shelf drain hole.

CombiFlash® Rf Installation Guide

5-4

5.4 Flow Cell Cleaning

5.4.1 Post Separation

As a preventive measure, all default column methods finish the separation run with a high percentage of solvent B (Figure 5-3). This brief time (two to three column volumes) of strong solvent flushes residual compounds from the column, flow cell, and internal tubing.

Figure 5-3 Default post-separation column and flow cell flush

Avoid skipping the flush by stopping the run after the last compound elutes. Skipping the flush may cause residual compounds to build up and crystallize, which might result in:

• cross contaminating later separation runs

• higher operating pressures

• reduced flow cell lamp energy

• a noisy baseline on the absorbance trace

• frequent messages recommending flow cell cleaning (Figure 5-4).

Allow the separation run to complete the full default column method. If the conditions above occur repeatedly, consider extending the flush time in the default column methods (Tools>Edit Defaults).

100

Gradient % Solvent B

Time or Column Volumes

Initial %B

Next Run Initial %B

End of

Separation

End of

Run

Flush

Separation

Gradient

Section 5 Maintenance

5-5

CAUTION

When using methanol as solvent B with silica column media, do not pump more than 50% solvent B. Higher percentages of methanol might break down the silica structure, possibly causing obstructions in the flow path.

5.4.2 Quick Cleaning when Recommended

When the lamp energy is lower than normal, the system will recommend flow cell cleaning (Figure 5-4) before starting a separation run.

Figure 5-4 Flow cell cleaning message

When the system displays this message you can:

• Cancel Run (recommended) – Click the Cancel Run button so you can perform a quick cleaning described in the following steps.

• Continue Collect All – Click this button to ignore the message. Because the peak detection operation might be impaired, the system automatically collects all fluids to avoid diverting compounds of interest to waste.

• Help – Click this button to display the flow cell cleaning on-line help topic.

To perform a quick cleaning:

1. After clicking the Cancel Run button, select the Tools>Manual Control menu option.

2. From the Manual Control window (Figure 5-5), note the Raw Lamp Energy level at 254 nm. The Raw Lamp Energy gauge has three ranges: red, yellow, and green.

CombiFlash® Rf Installation Guide

5-6

Figure 5-5 Raw Lamp Energy Gauge

• Red – lamp energy is obstructed to a degree that the system might not reliably detect peaks. If you attempt to operate the system, peak collection will be forced to collect all. This prevents diverting desired compounds to waste.

• Yellow – lamp energy is partially obstructed and the peak detector performance might be impaired. The system can be operated although the absorbance trace might appear noisy. Yellow might be a normal indication for systems with flow cell windows stained by compounds.

• Green – lamp energy is sufficient to detect peaks up to 3.0 Absorbance Units.

3. Remove the column and insert a bypass tube between the upper and lower column mounts. A bypass tube (P/N 209-0165-46) can be found in the accessory kit (P/N 60-5239-006).

4. Set the Flow Rate to 40 mL/min (Figure 5-6).

5. Select Through column for the Valve Position option.

6. Select Next for the Pump into Tube # option. By pumping into a collection tube, the diverter valve is also cleaned of any residue during this operation.

7. Click the Prime B button to pump 100% Solvent B through the bypass tube and into the collection tubes.

Section 5 Maintenance

5-7

Figure 5-6 Manual Control Settings - Quick Cleaning

Note

Pumping solvent B at a moderate flow rate (25 to 45 mL/min) over time will usually solubilize obstructions. Generally, the recommended solvent is the highest polarity solvent you have recently used (solvent B).

8. Monitor the Raw Lamp Energy gauge. As the system pumps solvent, the raw lamp energy should gradually improve. Pump solvent for two to five minutes or until the indicator reaches the far-right of the green range.

When the indicator is in the yellow, the lamp energy and flow cell are ready for the next run. However, continuing the cleaning for greater raw lamp energy should reduce the frequency of flow cell cleaning messages (Figure 5-4).

If after five minutes the indicator is still in the red range, repeat the cleaning steps using an alternative solvent (Table 5-1). Or, complete the steps in the Monthly Flow Cell Cleaning procedure (section 5.4.3).

Note

If the numerical values of the Raw Lamp Energy (Figure 5-5) do not change, or if the first number remains at zero, contact Teledyne Isco’s Technical Service department.

CombiFlash® Rf Installation Guide

5-8

Table 5-1 Suggested Flow Cell Cleaning Solvents

Solvent Description

Methanol Miscible with most LC solvents. Methanol will force other

solvents through the system so they will not interfere with the next sample. It breaks down the tertiary structure of silica and allows it to flush through.

Acetone Common organic solvent with high dissolving properties.

Acetone absorbs UV light at 254 nm. Therefore, the Raw Lamp Energy gauge will always read red when acetone is in the flow cell. After pumping acetone, pump a different solvent through the system to remove the acetone and read the Raw Lamp Energy gauge.

Dichloromethane (DCM)

Effective at solubilizing organic molecules.

Dimethylsulfoxide (DMSO)

Strong solvent that will clear organic sample.

Dimethylformamide (DMF)

Strong solvent if other solvents do not produce the desired results.

Tetrahydrofuran (THF)

Strong solvent.

Water/DMF/ methanol

A 50/25/25 solvent mixture effective in clearing some obstructions.

Water/DMF/ Acetic Acid

30/30/30ml solvent mixture effective in clearing some obstructions.

Mildly acidic aqueous solution

0.5M acetic acid in distilled water can be used to clear samples that are not removed by organic solvents.

Mildly basic aqueous solution

A dish-type detergent solution can wash through particulates not picked up by the acidic solution. The emulsification effect of detergent is an effective tool as well to help wash through oily samples. Follow the detergent with several minutes of clean, distilled water.

a. Recent synthesis solvents should also be considered.

Section 5 Maintenance

5-9

5.4.3 Monthly Flow Cell Cleaning

Perform this procedure as part of your scheduled preventive maintenance, or when Quick Cleaning As Required (section

5.4.2) does not improve the lamp energy.

1. Remove the column and insert a bypass tube between the upper and lower column mounts. A bypass tube (209-0165-46) can be found in the accessory kit (60-5239-006).

2. From the menu, select Tools>Manual Control. This opens the Manual Control window.

3. Set the Flow Rate to 40 mL/min (Figure 5-6).

4. Select Through column for the Valve Position option.

5. Select Next for the Pump into Tube # option.

6. Place the B1 Solvent inlet line into a reservoir of methanol, acetone, or a strong solvent that readily dissolves residual sample material.

7. Click the Prime B button to pump 100% Solvent B through the bypass tube and into the collection tubes.

8. After three minutes, click the Stop button. Allow the system to stand for at least six hours. Overnight is recommended.

9. Return the B1 solvent line to the original solvent container.

10.Perform the Quick Cleaning as Required (section 5.4.2) and monitor the Raw Lamp Energy.

If the lamp energy is in the green or yellow range, return the system to operation. If the lamp energy is red, contact Teledyne Isco’s Technical Service department for assistance.

CombiFlash® Rf Installation Guide

5-10

5.5 Electrical Troubleshooting

If your instrument stops working and the touch panel display is off, check the line cord connection.

If the line cord is connected properly, check the fuses in the power input module located on the system’s rear panel. These are time delay fuses (T-type) and rated according to the mains input power voltage:

• 100 to 129 VAC mains input: 2.0 A fuse

• 215 to 264 VAC mains input: 1.0 A fuse.

CAUTION

Always replace fuses with the same type and rating.

DECLARATION OF CONFORMITY

Application of Council Directive: 2004/108/EC -The EMC Directive

2002/96/EC – The WEE E Directive

73/23/EEC – The Low Voltage Directive

Manufacturer's Name: Teledyne Isco, Inc.

Manufacturer's Address: 4700 Superior, Lincoln, Nebraska 68504 USA

Mailing Address: P.O. Box 82531, Lincoln, NE 68501

Equipment Type/Environment: Laboratory Equipment for Light Industrial/Commercial Environments

Trade Name/Model No: CombiFlash Rf

Year of Issue: 2007

Sta

ndards to which Conformity is Declared: EN 61010-1 2nd edition Safety Requirements for Electrical Equipment for

Measurement, Control, and Laboratory Use

EN 61326-1:2006 EMC Requirements for Electrical Equipment for

Measurement, Control, and Laboratory Use

Standard Description Severity Applied Performance Criteria

EN61000-4-2 Electrostatic Discharge Level 2 - 4kV contact discharge

Level 3 - 8kV air discharge

EN61000-4-3 Radiated RF Immunity 80 MHz to 1000MHz 80% AM at 1kHz

Level 2 - 3V/m

EN61000-4-4 Electrical F

ast Transient Level 2 - 1kV on AC lines A

EN61000-4-5 Surge on AC Lines Level 2 - 1kV common mode,

Level 2 - 0.5KV differential mode

EN61000-4-6 Conducted RF on AC lines 150 kHz to 80 MHz,

Level 1 - 1V rms, 80% modulated

EN6100-4-11 Voltage Dips/Interruptions 100% drop, 10ms

CISPR11/ EN 55011

RF Emissions Group 1, Class A Industrial, Scientific, and

Medical Equipment

EN61000-3-2, 3-3 Harmonic and Flicker

We, the undersigned, hereby declare that the design of the equipment specified above conforms to the above Directive(s) and Standards as of April 12, 2007.

William Foster USA Representative

Teledyne Isco Inc.

William Foster

Director of Engineering Teledyne Isco, Inc. 4700 Superior Street Lincoln, Nebraska 68504

Phone: (402) 464-0231 Fax: (402) 464-4543

60-5232-141

Companion with Touchscreen Hazmat Table 60-5233-406 Rev.

Name and amount of Hazardous Substances or Elements in the product

Hazardous Substances or Elements

Component Name

(Pb) (Hg) (Cd) (Cr(VI)) (PBB) (PBDE)

LCD Display

O X O O O O

Circuit boards

X O O O O O

Wiring

O O O O X O

Internal Cables

O O O O X O

Line Cord

O O O O X O

Stepper Motor

X O O O X O

Deuterium lamp

O O X O O O

Valve Body

O O O O X O

Name and amount of Hazardous Substances or Elements in the product

ST/

O: Represent the concentration of the hazardous substance in this component’s any homogeneous pieces is lower than the

ST/ standard limitation.

ST/

( “X” )

X: Represent the concentration of the hazardous substance in this component’s at least one homogeneous piece is higher

than the ST/ standard limitation.

(Manufacturer may give technical reasons to the “X” marks)

The Environmentally Friendly Use Period (EFUP) was determined through experience.

(207 2007 ) A

The date of Manufacture is in code within the serial number. The first three numbers are the year of manufacture (207 is year 2007) followed by a letter for the month. "A" is January, "B" is February and so on.

Teledyne Isco One Year Limited Warranty*

Factory Service for Teledyne Isco CombiFlash® Systems

This warranty exclusively covers Teledyne Isco CombiFlash

instruments, providing a one-year limited

warranty covering parts and labor.

the customer will pay to return the instrument to Teledyne Isco, and Teledyne Isco will pay surface transportation to return the repaired instrument to the customer. Teledyne Isco will not pay air freight or customer’s packing and crating charges. This warranty does not cover loss, damage, or defects resulting from transportation between the customer’s facility and the repair facility.

Any instrument that fails during the warranty period due to faulty parts or workmanship will be repaired at the factory at no charge to the customer. Teledyne Isco’s exclusive liability is limited to repair or replacement of defective instruments. Teledyne Isco is not liable for consequential damages.

The warranty for any instrument is the one in effect on date of shipment. The warranty period begins on the shipping date, unless Teledyne Isco agrees in writing to a different date.

CombiFlash systems are designed to use Teledyne Isco RediSep columns. RediSep columns lead the industry in quality and performance. Customers may use other brands of columns on their CombiFlash instruments. These nonRediSep columns may fail to separate compounds, may leak silica into the flow path of the CombiFlash instrument, and may leak solvents from their fittings and seals.

Excluded from this warranty are normal wear; expendable items such as charts, ribbon, lamps, tubing, and glassware; fittings and wetted parts of valves; and damage due to corrosion, misuse, accident, or lack of proper maintenance. This warranty does not cover products not sold under the Teledyne Isco trademark or for which any other warranty is specifically stated.

Damage to CombiFlash instruments resulting from the failure of a non-RediSep column may cause the need for repairs that incur billable service activities. The customer is responsible for these charges.

This warranty is expressly in lieu of all other warranties and obligations and Teledyne Isco specifically disclaims any warranty of merchantability or fitness for a particular purpose.

Teledyne Isco will pay surface transportation charges both ways within the 48 contiguous United States if the instrument proves to be defective within 30 days of shipment. Throughout the remainder of the warranty period,

The warrantor is Teledyne Isco, Inc. 4700 Superior, Lincoln, NE 68504, U.S.A.

* This warranty applies to the USA and countries where Teledyne Isco Inc. does not have an authorized dealer. Customers in countries

outside the USA, where Teledyne Isco has an authorized dealer, should contact their Teledyne Isco dealer for warranty service.

Before returning any instrument for repair, please call, fax, or e-mail the Teledyne Isco Service Department for instructions. Many problems can often be diagnosed and corrected over the phone, or by e-mail, without returning the instrument to the factory.

Instruments needing factory repair should be packed carefully, preferably in the original carton, and shipped to the attention of the service department. Small, non-fragile items can be sent by insured parcel post. PLEASE BE SURE TO ENCLOSE A NOTE EXPLAINING THE DEFECT.

Shipping Address: Teledyne Isco, Inc. - Attention Repair Service

4700 Superior Street Lincoln NE 68504 USA

Mailing address: Teledyne Isco, Inc.

PO Box 82531 Lincoln NE 68501 USA

Phone: Repair service: (800)775-2965

(lab instruments)

(800)228-4373

(samplers & flow meters)

Sales & General Information (800)228-4373

(USA & Canada)

Fax: (402) 465-3001

Email: iscoservice@teledyne.com Web site: www.isco.com

February 1, 2006 P/N 60-2132-281 Rev C

Teledyne Installation Guide Installation Manual

Specifications and Main Features

Frequently Asked Questions

User Manual