S 4245 S4250 UV VIS Detektor HPLC Manual Schambeck SFD

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S 4245 UV/VIS DETECTOR

USER MANUAL

VERSION 1.0 (2012-10-25)


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TABLE OF CONTENTS
Contents 5.3.3 Submenu: Basic Settings  Wavelength Program 24
5.3.4 Submenu: Deuterium Lamp Status 25
1. Introduction 5 5.3.5 Submenu: System 26
1.1 How to Use this Manual 5
1.1.1 Symbols 5 6. Instrument Operation 27
1.2 Safety Information 6 6.1 Overview 27
1.2.1 General Safety Information 6 6.1.1 Internal Mode 27
1.2.2 Intended Purpose 6 6.1.2 External Mode 27
1.2.3 Environmental Safety 6 6.1.3 Serial Mode 27
1.2.4 Electrical Safety 6 6.2 Instrument Initialization 27
Step 1: Status - Init 27
2. Instrument Overview 9 Step 2: Status - Calib 27
2.1 General Instrument Overview 9
6.3 Manual Operation (Internal Mode) 28
3. Instrument Description 11 6.4 Remote Operation (External Mode) 29
3.1 General Instrument Description 11
3.1.1 Front Panel Description 11
7. Instrument Maintenance 31
3.1.2 Back Panel Description 13 7.1 Flowcell 31
7.1.1 Flowcell Assembly 31
3.2 Functional Description 14
3.2.1 Front Elements 14 7.2 Deuterium & Tungsten Lamps 32
3.2.2 Functional Elements 15 7.2.1 Lamp Exchange 32
3.2.3 Principle of Operation 16 Appendix A: Specifications 33
4. Instrument Setup 17 A.1 Technical Specifications 33
4.1 Unpacking 17 A.2 Environmental Conditions 34
4.2 Capillary Connections 17 A.2.1 Operational Conditions 34
A.2.2 Storage Conditions 34
4.3 Backside Connections 18
4.3.1 Electrical Connections 18 Appendix B: Accessories 35
5. Instrument Menus 19 B.1 Standard Accessories 35
5.1 Keyboard 19 Appendix C: Version Control 37
5.2 Status Screen 20 C.1 Version History 37
5.3 Menu Description 21
5.3.1 Submenu: Basic Settings  General 22
5.3.2 Submenu: Basic Settings  Analog Output 23

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1. INTRODUCTION
1.1 How to Use this Manual
This manual is designed as a reference to the installation, operation and
maintenance of the S 4245 UV/Vis Detector.
It is strongly recommended to review this manual before operating the in-
strument.
The content of this manual is subject to change without notice. This docu-
ment is believed to be complete and accurate at the time of publication.
The Manufacturer is not liable for any damage resulted from the use of this
manual.

1.1.1 Symbols
Throughout this manual important text sections are marked with the fol-
lowing symbols:

This section includes important information which may result in in-


strument or personal damage if not carefully followed.
STOP !

This section includes important information for the proper opera-


tion of the instrument. Failure to follow this information may result in ! WARNING
faulty behaviour of the instrument and/or wrong analysis results.

This section emphasis some detailed information intended to optimize


the performance of the instrument or to give a better understanding of
NOTE
some technical details.

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1.2 Safety Information
This instrument is compliant with all related standards as stated in Ap-
pendix B.

1.2.1 General Safety Information


The operation of any analytical instrumentation requires the operator to be
familiar with the potential hazards of using chemical solvents.
To avoid personal injury and/or damage to the instrument the operator is
responsible to follow all safety information herein.
The manufacturer assumes no liability for any damage resulted from not
following any of these safety procedures.

1.2.2 Intended Purpose


This instrument is designed and certified as a general purpose laboratory
instrument for research and routine analysis work only. It is not certified
for in-vitro or other medical applications.
Any use outside this intended purpose does not fall with the manufactur-
er’s liability.

1.2.3 Environmental Safety


Only operate the instrument in well-ventilated areas. If volatile or flam-
mable solvents are used with this instrument, arrange for proper disposal
of any waste and/or fumes.
Always properly dispose any waste solvents.
Avoid open flames and sparks when working with flammable and volatile
solvents.
In case of instrument leakage, turn off the instrument and remedy the leak-
age problem immediately.

1.2.4 Electrical Safety


Always use the provided power cords.

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Replace faulty power cords and other cables before operating the instru-
ment.
Always replace blown fuses with original spare fuses.
When the instrument’s housing is open, electrical connections will be ex-
posed. Disconnect the instrument from the main power before opening
the housing.

The housing should only be opened by certified service personnel!


Damage of the instrument of injury may result from improper han-
STOP !
dling.

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2. INSTRUMENT OVERVIEW
2.1 General Instrument Overview
The S 4245 UV/Vis Detector is a variable wavelength UV/Vis detector for
routine analysis and sophisticated research. The dual lamp design offers
a wavelength range of 190 – 800 nm with a low baseline noise. The front-
accessible flowcell can easily be exchanged, as can be the lamps which are
accessible through a side panel in the instrument housing.

Integrated Wavelength Program


The S 4245 UV/Vis Detector features a wavelength program to change the
selected wavelength over time. With this feature the optimum wavelength
can be selected for each analyzed substance according to its retention time.

Integrated Peak Detector


The integrated Peak Detector works as a basic fraction collector. The peak
detection level can be freely programmed for peak start and peak end to
enhance the collection purity. An integrated 24V output for switching a
solenoid valve is used for the fraction collection, which is automatically
operated with a selectable time delay.

[mV]

20.0

10.0
Peak End Detection Level

Peak Start Detection Level

0.0
Peak Start Peak End
Time Time
0.0 1.0 2.0 Solenoid 3.0
Valve OFF

+Delay
Fraction Collection

+Delay
Solenoid
Valve ON

Figure: S 4245 Peak Detector

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Optional – Dual-Wavelength
The S 4245 UV/Vis Detector is available with an optional second wave-
length. This feature enhances the Wavelength Program feature that you can
measure 2 different wavelengths at the same time. A second D/A converter
output comes with this option to keep the system flexible to be used with
any data acquisition software available.

Optional – Online-Scan
Another option for the S 4245 UV/Vis Detector is the Online Scan. With
the Online Scan whole spectrum information can be gathered at a certain
time. This scan information is stored internally and can be accessed at any
time. The Online Scan is a good alternative to a full UV PDA detector.

Figure: S 4245 Optical Module

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3. INSTRUMENT DESCRIPTION
3.1 General Instrument Description
3.1.1 Front Panel Description
The front panel of the S 4245 UV/Vis Detector consists of three main ele-
ments: the TFT Display (1), the Keyboard (2) and the Front Cover (3).
The 3” TFT Display shows the current status information and is used with
the Keyboard to adjust instrument settings and fully operate the instru-
ment in stand-alone mode without a PC required.
The Front Cover has a view panel, so that the important parts are always
visible to the operator. In case of a leak it can be detected before solvents are
leaking out of the bottom of the Front Cover.
The Front Cover can be opened to easily access the flowcell.

# Element
1 TFT Display
2 Keyboard
3 Front Cover

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Removing the Front Cover
The Front Cover of the S 4245 UV/Vis Detector is completely removable
at its hinges.
• Open The Front Cover to 90° (in order to get free of any instrument
stacked on top)

• Remove the Front Cover


• Store the Front Cover at a safe place

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3.1.2 Back Panel Description
The back panel of the S 4245 UV/Vis Detector houses the power and inter-
face connectors and several drain outlets.
The Power Cord Connection & Power Switch housing holds the main fuse
in an internal fuse carrier.
The digital I/O and other interface connectors are used for remote instru-
ment control and are discussed in a later chapter.

# Element
1 Instrument Serial Number
2 Power Cord Connection &
Power Switch
3 Remote Digital I/O Connector
4 RS-232 Interface Connector
5 RS-485 Interface Connectors
6 USB Interface Connector

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3.2 Functional Description
3.2.1 Front Elements
The S 4245 UV/Vis Detector has all important parts directly accessible
from the front panel when the Front Cover is opened or removed.
The Capillary Holder (3) holds the pump inlet capillary in place.
The flowcell (4) is completely accessible from the front to make capillary
connections to the flwcell inlet (5) and outlet (6) and can be easily removed
with 2 screws..

# Element
1 TFT Display
2 Keyboard
3 Capillary Holder
4 Flowcell
5 Flowcell Inlet
6 Flowcell Outlet

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3.2.2 Functional Elements
All functional elements of the S 4245 UV/Vis Detector are located inside
the instrument.
The Display PCB (1) controls the TFT Display and Keyboard. It is acces-
sible when the display panel is removed.
The Lamp Power Supply Unit (2) supplies the required voltage and ignition
sequence for the Deuterium lamp.
The Power Supply Unit (3) supplies 24V to the PCB’s. The input voltage is
variable from 90 V to 240 V (5).
The Controlled PCB (4) controls the whole pump.
The Fan (6) is mounted on the back panel and is important for regulating
the internal temperature.
The Lamp Connector Rack (7) is used for easy connection of Deuterium
and Tungsten lamps from the side panel of the instrument.

# Element
1 Display PCB
2 D2-Lamp Power Supply
3 24V Power Supply Unit
4 Controller PCB
5 Mains Connector
6 Fan
7 Lamp Connector Bracket
8 Optical Module

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3.2.3 Principle of Operation

Reference
Signal

2nd Order
Filter

Measuring Signal

Beam
Splitter Flow
Cell
Grating

Deuterium
Lamp

Tungsten
Lamp

Figure: Principle of Operation

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4. INSTRUMENT SETUP
4.1 Unpacking
Remove the S 4245 UV/Vis Detector from its package and put it on the
working desk. Check the instrument thoroughly for any damage that may
have occurred during shipping. Contact your supplier in case of any dam-
ages.
Check the accessories shipped with the instrument if everything is com-
plete and in good condition.

4.2 Capillary Connections


Connect the capillary coming from the separation column to the flowcell
inlet (4). Then connect the drain capillary to the flowcell outlet (3).

# Element
1 Capillary Holder
2 Flowcell
3 Flowcell Outlet
4 Flowcell Inlet

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4.3 Backside Connections
4.3.1 Electrical Connections
• Connect the supplied power cord to the Mains connector (2).
• Connect the supplied RS-232 cable to the RS-232 connector (4) if
the instrument is to be operated by PC
• Connect the remote control wires to the Digital I/O connector (3) if
the instrument is to be run in External mode.
Please refer to 5. Instrument Operation for further information about PC
control and Remote control.

# Element
1 Serial Number
2 Mains connector
3 Remote Digital I/O
4 RS-232 Serial Communication
5 RS-485 Communication Bus
6 USB Communication
(not in use)

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5. INSTRUMENT MENUS
5.1 Keyboard
The S 4245 UV/Vis Detector parameters can be adjusted at any time via the
screen menu and keyboard on the front panel.

[MENU] Key
With the [MENU] key you can access the Main Menu and select a sub-
menu.

[STATUS] Key
With the [STATUS] key you can access the status screen from any menu.

[EDIT] Key
Use the [EDIT] key to change any parameters. When you press the [EDIT]
key, the selected parameter can be changed. Confirm the new setting by
pressing the [EDIT] key again.

[CANCEL] Key
With the [CANCEL] key you can abort the change of a parameter. When
pressing [CANCEL] key instead of [EDIT] key when changing a param-
eter, the change is discarded and the original value is used.

[CURSOR] Keys
The 4 arrow [CURSOR] keys are used to navigate the menus.

[ZERO] Key
The [ZERO] key sets the baseline absorption value to zero.

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[PROG] Key
The [PROG] key starts the wavelength program.

5.2 Status Screen


The Status Screen shows the most important parameters.

Mode
The top line shows the currently selected mode: Intern, Extern or Serial.

Status
On the top right the current status is displayed: Init, Calib, Ch1, or Ch2

Wavelength
The currently selected wavelength.

Absorption
The current absorption at the selected wavelength.

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5.3 Menu Description
With the [MENU] key, the Main Menu is displayed.
Use the [CURSOR] key ([UP] and [DOWN]) to browse through the Main
Menu for access of one of the Submenus.

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5.3.1 Submenu: Basic Settings  General

Ch1 Wavelength
Select the desired wavelength for Channel-1 from 190 to 800 nm.

Ch2 Wavelength (optional)


Select the desired wavelength for Channel-2 from 190 to 800 nm.

Ch1 Rise Time


Select the desired Rise Time for Channel-1. The Rise Time is a electronic-
noise reduction, where a higher value results in higher noise reduction-

Ch2 Rise Time


Select the desired Rise Time for Channel-2. The Rise Time is a electronic-
noise reduction, where a higher value results in higher noise reduction-

Detector Lamps
Select which lamps should be used for normal operation.

Multi-Channel Mode
Select the desired channel mode: single channel or dual-channel (optional).

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5.3.2 Submenu: Basic Settings  Analog Output

Ch1 Range
Select the Range for Channel-1. The Range specifies the AU output scaled
to a 1 V analog signal.
Ch2 Range
Select the Range for Channel-2. The Range specifies the AU output scaled
to a 1 V analog signal. (optional)

Ch1 Offset
Select an Offset for Channel-1’s analog signal.

Ch2 Offset
Select an Offset for Channel-2’s analog signal. (optional)

Peak Detector Threshold


Select the Peak Detection Threshold for detecting peaks. If this threshold
is reached, a 24V output (solenoid valve) is activated to collect a fraction
of this peak.

Peak Delay
Select a delay for the Peak Detector. This time delay should be equal to the
time the sample needs to move from the detector’s flowcell to the solenoid
valve.

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5.3.3 Submenu: Basic Settings  Wavelength Program

#
The step-number of this row.

Time [min]
The time when this wavelength program step activates.

λ [nm]
Select the new wavelength for this step.

Action
Select between AZ, OFF, or None.
AZ: execute an Autozero at the beginning of this step.
OFF: calculate a baseline-offset between the latest signal and ne new sig
nal of this step.
None. do nothing after changing the wavelength.

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5.3.4 Submenu: Deuterium Lamp Status

D2 Runtime
Shows the total runtime of the deuterium lamp in hours.

D2 Total Ignitions
Shows the total number of ignitions of the deuterium lamps since reset.

D2 Energy
Shows the current lamp energy in %.

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5.3.5 Submenu: System

System Int./Ext./Serial
Display Version
Mainboard Version
GLP 24V
GLP 5V
Int./Ext./Ser.
The Operation Mode can be changed here between Intern, Extern or Serial.

Display Version
The Software Display is the installed firmware version of the Display PCB.

Mainboard Version
The Software Display is the installed firmware version of the Controller
PCB.

GLP 24V
The +24V Voltage is an actual voltage reading for one of the PCB’s con-
trolled voltages.

GLP 5V
The +5V Voltage is an actual voltage reading for one of the PCB’s controlled
voltages.

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6. INSTRUMENT OPERATION
6.1 Overview
The S 4245 UV/Vis Detector can be operated in 3 different Operation
Modes: Internal, External, or Serial

6.1.1 Internal Mode


In Internal Mode the instrument is controlled manually with the Keyboard.

6.1.2 External Mode


In External Mode the instrument is controlled via the Remote Digital I/O
contacts.

6.1.3 Serial Mode


In Serial Mode the instrument is controlled by a PC software (e.g. Clarity)
via RS-232 serial line.

6.2 Instrument Initialization


When the S 4245 UV/Vis Detector is switched on it goes through a number
of initialization steps. These steps are outlined below:

Step 1: Status - Init


The detector measures its dark current and check the lamps.

Step 2: Status - Calib


After the initialization, the detector calibrates its wavelength. This takes
some time as the grating has to be moved through the whole spectrum to
calibrate itself.

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6.3 Manual Operation (Internal Mode)
The S 4245 UV/Vis Detector can be operated manually.
When the instrument is in Internal mode, the detector measures continu-
ously

6.3.1 Autozero
Press [ZERO] key on the front panel to execute autozero.

6.3.2 Wavelength Program


Press [PROG] to start the wavelength program if the program key is cur-
rently assigned to the wavelength program.

6.3.3 Online Scan


Press [PROG] to start the online scan if the program key is currently as-
signed to the online scan. The scan replay is also started with the [PROG]
key if assigned to the replay function.

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6.4 Remote Operation (External Mode)
Some functions of the S 4245 UV/Vis Detector can be operated exter-
nally.
REMOTE Pin Function
Please refer to the Remote Connector layout on the right (NOTE: Pin 1 Channel-1 GND
1 of the connector directly faces the RS-232 connector). 2 Channel-1 Signal
3 Channel-2 GND
The REMOTE START function corresponds to the [Start] key on the
4 Channel-2 Signal
front panel and can either start the wavelength program or online
5 Error Output GND
scan.
6 Error Output
7 GND
8 not used
9 GND
10 REMOTE START
11 GND
12 Valve (+24 V Output)

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7. INSTRUMENT MAINTENANCE
7.1 Flowcell
7.1.1 Flowcell Assembly
The following diagram shows all the components of the dismantled flow-
cell:

# Element
1 Holding Screw (SS)
2 Centering Disc (PEEK)
3 Quartz Lens
4 PTFE Sealing

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7.2 Deuterium & Tungsten Lamps
7.2.1 Lamp Exchange
The lamps can be accessed from the left side panel of the instrument.
• Remove the side panel to access the lamps

# Element
1 Deuterium Lamp
2 Tungsten Lamp
3 Tungsten Lamp Conector
4 Deuterium Lamp Connector

Exchange Deuterium Lamp


After opening the side panel, the Deuterium Lamp can be accessed.
• remove the Deuterium Lamp by loosening the top and bottom
screw (1)
• disconnect the Deuterium Lamp (4)
Now, the Deuterium Lamp can be removed and a new lamp inserted.

Exchange Tungsten Lamp


After opening the side panel, the Tungsten Lamp can be accessed.
• remove the Tungsten Lamp by loosening the PEEK finger-screw on
top of the Tungsten Lamp housing (2)
• disconnect the Tungsten Lamp (3)
Now the Tungsten Lamp can be removed and replaced by a new lamp.

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APPENDIX A: SPECIFICATIONS
A.1 Technical Specifications
Wetted Materials: Stainless Steel / PEEK*, PTFE, Quartz
Baseline Noise: ± 1 x 10-5 AU (@240nm, 2 sec Risetime)
Baseline Drift: < 3 x 10-4 AU/h
Wavelength Range: 190 - 800 nm
Wavelength Accuracy: ± 2 nm
Linearity > 2.0 AU
Light Source: Deuterium Lamp, Tungsten Lamp
Wavelength Program: Programmable, 10 steps
Analog Output 1x 1 V (optional: 2x 1 V)
Control Features: Internal Peak Detector with 24V solenoid
switching output
Dimensions: 310 x 165 x 478 mm (W x H x D)
Weight: 7.0 kg
Power Supply: 100 – 250 ~V, 47 – 63 Hz
* depending on material option

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A.2 Environmental Conditions
A.2.1 Operational Conditions
Ambient Temperature: +10 °C to +35 °C
Ambient Relative Humidity: 20 to 80 % RH (non-condensing)

A.2.2 Storage Conditions


Ambient Temperature: -20 °C to +60 °C
Ambient Relative Humidity: 20 to 80 % RH (non-condensing)

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APPENDIX B: ACCESSORIES
B.1 Standard Accessories
The S 4245 UV/Vis Detector is delivered with the following standard ac-
cessories:
• 1x Power Cord (EU Type)
• 1x Serial Cable (RS-232)
• 1x 1/16” Drain Capillary, FEP (I.D. 0.8mm, 2 m)
• 1x 1/16” Fitting & Ferrule, Stainless Steel
• 1x Operation Manual (this)
• 2x Fuse, 2 A

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APPENDIX C: VERSION CONTROL
C.1 Version History
The S 4245 UV/Vis Detector Operation Manual is subject to version control.
The version history is continued and noted on every document. The access
to the original document is restricted to the creating party. The document
is subject to periodical checks and can never reach an unchangeable state.
Version Release Date Description
1.0 2012-12-03 First Release

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