Teledyne Installation Guide Installation Manual

i

CombiFlash® R

f

Installation Guide

For indoor use only

COPYRIGHT © 2002, 2004 by
Teledyne Isco, Inc.
4700 Superior St., Lincoln, Nebraska, U.S.A. 68504

Phone: [phone]
Toll Free: [phone]
FAX: [phone]

Revision A: August 15, 2007

Part #60-5233-385

iii

CombiFlash® R

f

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

iv

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

f

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

f

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

f

, 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

f

system at the instrument,

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

The CombiFlash R

f

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

f

can purify samples

from 4 milligrams to greater than 33 grams using RediSep R

f

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

f

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

f

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

f

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

f

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

1

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

f

.

Figure 1-2 CombiFlash R

f

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.

3

4

1

5

6

7

8

9

10

2

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

f

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

f

Features (Back)

11

12

19

20

23

16

13

14

15

22

21

18

24

17

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: [phone] or [phone]
Fax: [phone]
E-mail: [e-mail]

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

f

Installation Guide

Section 2 System Preparation

This section provides instructions for unpacking and installing
the CombiFlash R

f

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

2

) of level bench space.

Ensure that the CombiFlash R

f

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

f

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

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

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.