Schambeck RI 2000 User manual

RI 2000

Version 1.1
Printed: 09.07.2014
File: RI2000 V4.0 SFD English FINAL 07-2014.doc
Last modified: Makowski

Schambeck SFD GmbH Refractive Index Detector RI2000
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TABLE OF CONTENTS
TABLE OF CONTENTS 1
1CONTACT ADDRESS 3
2PRECAUTION AND WARNINGS 4
3ELECTRICAL WARNINGS 4
4GENERAL WARNINGS 5
5SPECIFICATIONS 7
6PHYSICAL SPECIFICATIONS 8
7GUARANTEE CONDITIONS 9
8PARTS INCLUDED IN THE DELIVERY 10
9FRONT PANEL AND KEYBOARD 11
9.1 THE DISPLAY 11
9.2 THE AUTOZERO BUTTON 12
9.3 THE PURGE BUTTON 12
9.4 THE BUTTON POL +/- 12
9.5 THE BUTTONS ARROWLEFT (◄) AND ARROWRIGHT (►) 12
9.6 THE BUTTONS ARROWUP (▲) AND ARROWDOWN (▼) 12
9.7 THE MENU BUTTON 13
9.8 THE ENTER BUTTON 13
9.9 THE IN PORT 13
9.10 THE OUT PORT 13
10 THE BACK SIDE OF THE RI2000 14
10.1 OUTPUT-CONNECTORS 14
10.1.1 THE INTEGRATOR SIGNAL OUTPUT 14
10.1.2 THE RECORDER SIGNAL OUTPUT 14
10.1.3 THE DIGITAL OUTPUT 14
10.2 INPUT-CONNECTORS 15
10.2.1 THE EXTERNAL START SIGNAL 15
10.2.2 THE EXTERNAL AUTOZERO SIGNAL 15
10.2.3 THE EXTERNAL PURGE SIGNAL 15
10.3 THE RS232 PORT 15
10.4 MASS SCREW 15
10.5 OPTICAL ADJUST 16
10.6 DRAIN 16
10.7 MAINS ADAPTOR 16
10.8 FUSES 16
11 INSTALLATION OF THE RI2000 17
11.1 CONNECTING THE DETECTOR TO THE CHROMATOGRAPHY SYSTEM 17
11.2 CONNECTION TO AN ANALOG DATA SYSTEM 18
11.3 CONNECTION TO A DIGITAL DATA SYSTEM (PC) 18
12 PRINCIPLE OF DETECTION 19
12.1 THE OPTICAL SYSTEM OF THE RI2000 19

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13 FLOW PATHS IN THE RI2000 20
13.1 MEASURING MODE WITH MTV –VALVE OR ASCO VALVE 20
13.2 PURGE MODE WITH MTV –VALVE OR ASCO VALVE 21
14 OPERATING THE RI2000 DETECTOR 23
14.1 OVERVIEW FIRMWARE VERSION 3.2C23
14.2 THE INITIALIZATION STAGE 24
14.3 THE NORMAL MEASURING MODE (NORMMODE) 25
14.4 TEMPERATURE SETTINGS 27
14.5 SETTING SIGNAL SMOOTHING 29
14.6 SETTING RECORDER RANGE –SIGNAL AMPLIFICATION 30
14.7 SETTING RECORDER OFFSET AND RECORDER EXTENT 31
14.7.1 RECORDER OFFSET 31
14.7.2 RECORDER EXTENT 32
14.8 MARKERS 33
14.9 SETTINGS FOR SERIAL PORT (RS232) 34
14.10 MENU STRUCTURE IN NORMAL MEASURING MODE (NORMMODE) 35
15 THE SERVICE MODE 36
15.1 FIRMWARE INFORMATION 37
15.2 VIEWFINE MODE 38
15.3 ADJUSTING DIGITAL –ANALOG –CONVERTERS 40
15.4 CALIBRATING THE RI2000 41
15.4.1 HOW TO CALIBRATE…42
15.5 SERVMODE OVERVIEW 45
15.6 SERIAL COMMUNICATION 46
16 MAINTENANCE OF THE RI2000 47
16.1 IDENTIFYING HARD-AND SOFTWARE 47
16.2 ERROR MESSAGES 48
16.2.1 MALFUNCTION OF THE TEMPERATURE SENSOR 48
16.2.2 MALFUNCTION OF THE ANALOG DIGITAL CONVERTER 49
16.2.3 INTENSITY ALARM OR SIGNAL#TOO LOW /SIGNAL#TOO HIGHT 50
16.2.4 SIGNAL OUT OF RANGE 51
16.2.5 RESET CONFIGURATION 52
16.3 ADJUSTING THE OPTICAL SYSTEM 53
16.4 LAMP EXCHANGE AND ADJUSTMENT OF THE LAMP 55
16.5 CHECKING SUM-AND DIFFERENCE VOLTAGES 59
16.6 CHECK AND REPLACEMENT OF THE VALVE 62
16.7 CHECKING AND CLEANING THE FLOW CELL 63
16.8 THE HEATING CIRCUIT OF THE RI2000 65
17 VOLTAGE TEST POINTS 66
18 SPARE PARTS 67
19 TEST POINTS FOR LAMP VOLTAGE (FOR SERIAL NUMBER 0312XXX) 68
20 TEST POINTS FOR LAMP VOLTAGE (FOR SERIAL NUMBER 0401XXX) 69
21 VOLTAGE TEST POINTS (OVERVIEW) FOR 0312XXX SERIES 70
22 VOLTAGE TEST POINTS (OVERVIEW) FOR 0401XXX SERIES 71
DECLARATION OF CONFORMITY 72

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1 CONTACT ADDRESS
In case of problems with your RI2000 refractive index detector please contact your local
distributor or Schambeck SFD GmbH.
Schambeck SFD GmbH
Rhöndorfer Strasse 51
D –53604 Bad Honnef
Germany
Telephone: [phone]
Telefax: [phone]
http://www.schambeck-sfd.com
Email: [email protected]

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2 PRECAUTION AND WARNINGS
The manufacturer is not reliable for any damage, harm or financial loss caused
directly or indirectly by the use of this instrument if the instrument is handled without
the observation of this manual or handling with carelessness.
■NOTE
Please read this manual carefully before working with the RI2000 refractive index detector.
In case of any question please do not hesitateto contact you local distributor or Schambeck
SFD GmbH directly.
3 ELECTRICAL WARNINGS
Before opening the housing of the instrument make sure the detector is switched off
and disconnected from power supply.
The voltage selected at the fuse on the backside of the instrument has to be set
correctly to 110 V or 220 V according to your local power supply.
Before changing the selected voltage the power supply has to be disconnected.
The detector may only be connected to plugs with grounding.
The RI2000 may only be operated in connection with other devices which fit to the
safety requirements.

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4 GENERAL WARNINGS
To prevent damages of the RI2000 all capillaries and cables have to be checked for
damages and leakages.
For the disposal of inflammable and/or toxic solvents a plan for waste management
has to be created. Such solvents may not get into the drain.
The RI2000 refractive index detector is built to operate at temperatures between
10 °C and 35 °C.
To reach a reliable operation of the detector it is recommended to use filtered
samples and solvents only.
The detector may be cleaned with appropriate cleaning agents only.
Make sure that no liquid gets inside the detector. Liquid inside the housing may
cause electrical short circuits which may result in the damage of the instrument.
To prevent electrical shocks make sure that the detector is disconnected from power
supply when the housing is opened to perform service work inside.
To disconnect the instrument from power supply simply unplug the power cable.
Electronic circuit boards and electronic components are sensitive to electrostatical
charges.
For some maintenance operation it is required to open the instrument’s housing.
Make sure that the instrument is disconnected from power supply before removing
the housing. It it is necessary to remove the housing during operation make sure not
to touch electrical parts inside the detector.

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In case of the use of dangerous solvents pay attention to safety instructions
regarding this solvent.
Solvents should be degassed before use with a refractive index detector.
After use of salt containing solvents (such as buffers) the detector should be purged
with distilled water.
Make sure that the 6 bar (0.6 MPa) pressure limit of the flow cell is not exceeded.
Make sure that the 2 bar (0.2 MPa) pressure limit of the valve is not exceeded.
During operation the housing of the detector should be closed.
Do not use the detector in ambience of aggressive gases, very high humidity, strong
vibrations and strong changes in the ambience’s temperature.

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5 SPECIFICATIONS
Type of detection:
Refractive Index
Effective range for refractive index:
1.00 –1.75 RIU
Effective range:
1000 µRIU
Optical null balance:
In the whole effective range by adjusting
the mirror
Signal null balance:
In the whole effective range by using the
AutoZero function
Materials which contact the mobile phase:
Stainless steel, glass, PTFE
Maximum pH-range:
2.3 –9.5
Temperature control for optical bench:
7°C above ambient temperature,
35 °C up to 55 °C in 1 °C steps
Analog signal output:
Recorder / integrator
Noise (analog signal):
10 nRIU (10 µV)
Noise (digital output):
5 nRIU ( 5 µV)
Drift:
< 1 µRIU/h (< 1mV/h)
Integrator output:
1.2 V (fix)
Recorder output:
1.2 V (adjustable)
Recorder range:
8 steps selectable in region from 1/8 to
16/1
Recorder offset:
Selectable: 0 mV, 10 mV, 100 mV
Signal range (recorder):
Selectable: 10 mV, 100 mV, 1000 mV
Recorder marker:
Marker function ON/OFF
Flow cell:
Glass cell (quartz) with two chambers
Volume:
9 µL
Angel:
45 °
Max. Pressure:
6 bar (0.6 MPa)
Max. Flow rate:
0.1 –3.0 mL/min
Valve:
3/2 path valve, 12 V
Max. Pressure:
2 bar (0.2 MPa)
Volumes:
Sample entry sample cell: 24 µL
Sample entry sample cell reference
cell sample exit: 1500 µL
Communication:
Digital interface: RS232, bidirectional
Digital input: TTL (Purge, AutoZero,
Start/Marker)
Digital output: TTL (Intensity alarm)

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6 PHYSICAL SPECIFICATIONS
Dimensions: 220 mm * 165 mm * 350 mm (W * H * D)
Weight: 12 kg
Voltages: Mains adaptor with voltage selector
100 –120 V
220 –240 V
Frequency: 50 or 60 Hz
Power consumption: max. 50 W
Temperature range: 10 °C to 50 °C

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7 GUARANTEE CONDITIONS
The term of guarantee depends on you local law. Beside this Schambeck SFD GmbH
affords guarantee for at least 12 months beginning after purchase of the RI2000 refractive
index detector.
All instruments are tested and certified by Schambeck SFD GmbH quality control.
Only defects which result from faulty manufacture or material defects are covered by the
guarantee. In case of a defect the original sales slip will be needed to make use of the
guarantee. Repair works covered by the guarantee may only be performed by Schambeck
SFD GmbH or licensed distributors.
The following cases are not covered by the guarantee:
Improper use (e. g. capacity overload, use of not approved tools) of the RI2000
detector
Parts which are liable to aging or abrasion like lamps, valves, heater cartridges or
flow cells
Damages caused by use of force or not approved tools
Damages which result from improper use due to non-observance of the operation
manual, the use under abnormal conditions or improper maintenance
Defects resulting from the use of third-party parts which are not approved by
Schambeck SFD GmbH
Instruments which are modified after purchasing by the customer
Normal abrasion
Fully or partial disassembled refractive index detectors

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8 PARTS INCLUDED IN THE DELIVERY
Quantity Description
1 EA Refractive Index Detector RI2000
1 EA Stainless steel capillary, 0.25 mm inner diameter,
1.59 mm outer diameter (for sample entry)
1 EA PTFE tube, 0,80 mm inner diameter,
1.59mm outer diameter (for sample exit)
2 EA Screw connection (for sample entry and sample exit)
1 EA Power cable
2 m Signal cable, 2-wired
1 EA RS232 cable
2 EA Fuses (0.5 A, slow for 220 V) or ( 1,0 A, slow for 110V)
1 EA Hex-wrench (for adjustment of the mirror, 2.5 mm)
1 EA Operation Manual on CD

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9 FRONT PANEL AND KEYBOARD
9.1 THE DISPLAY
The RI2000 refractive index detector is equipped with a liquid crystal display to show the
current detector signal as well as system parameters. This display contains four lines with
20 characters each.
Line 1 shows the current temperature of the optical bench (in °C).
Line 2 shows the optical balance (in %%).
Line 3 shows the current detector signal (in mV).
The value shown here is identical to the digital output signal and
to the analog signal which can be recorded at the recorder output.
Line 4 This line shows the status of the RI2000 detector.
Every few seconds the displayed parameter changes.
By this you can get a complete overview of all parameters in
a short time.

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9.2 THE AUTOZERO BUTTON
By pressing the AutoZero button the detector signal is internally set to Zero. To return to
the formel (unmodified) signal, press the AutoZero button for approx. three seconds.
9.3 THE PURGE BUTTON
To flush the reference chamber of the flow cell with mobile phase press the PURGE button
once. If the purge mode is activated a red LED will light up. Press the PURGE button once
again to deactivate the purge mode. Now the mobile phase will flow only through the sample
chamber of the flow cell.
9.4 THE BUTTON POL +/-
By pressing this button the polarity of the detector signal will be changed. A negative signal
like e. g. –5mV will be transformed into a positive signal + 5 mV when the polarity mode is
activated. A red LED will light up when this mode is activated.
9.5 THE BUTTONS ARROWLEFT (◄)AND ARROWRIGHT (►)
This arrow buttons have several functions. If only one button is pressed you can change
the settings of one parameter to smaller (◄) or bigger (►) values. If both buttons are
pressed together for about three seconds the detector will be set to the service mode.
9.6 THE BUTTONS ARROWUP (▲)AND ARROWDOWN (▼)
If different options for one parameter are available you can select the desired option by
using these arrow buttons. ArrowUp (▲) will switch to higher values and ArrowDown (▼)
to smaller values.
If the marker function is activated you can send a marker signal to the recorder output by
pressing the ArrowUp (▲) button (see chapter 14.8).

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9.7 THE MENU BUTTON
By pressing this button you can select a special sub menu or discard changes you
performed on a parameter.
9.8 THE ENTER BUTTON
Press the ENTER button to open the selected sub menu and to accept changes you
performed on a parameter.
9.9 THE IN PORT
This is the entrance for the mobile phase coming from the column. Connect the capillary
coming from the column to this port using screw connectors.
9.10THE OUT PORT
This is the exit of the mobile phase. Connect you waste bottle to this port using the PTFE
tube.
■NOTE
Use only capillaries with an inner diameter of 1 mm for the exit of the mobile phase. By
this blockage can be prevented. Make also sure that the pressure limits for the flow cell
(6 bar, 0.6 MPa) and the valve (2 bar, 0.2 MPa) are not exceeded.

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10 THE BACK SIDE OF THE RI2000
10.1OUTPUT-CONNECTORS
The RI2000 refractive index detector has two analog and one digital signal output.
10.1.1 THE INTEGRATOR SIGNAL OUTPUT
If you want to record your data using an analog integrator device, connect the integrator
using a shielded signal cable to the integrator output (Int. Out).
Make sure that the polarity (+/-) is correct.
10.1.2 THE RECORDER SIGNAL OUTPUT
To record data using an analog recorder, connect the device using the shielded signal cable
to the recorder output (Rec. Out). Make sure that the polarity (+/-) is correct.
10.1.3 THE DIGITAL OUTPUT
The RI2000 gives a TTL pulse in case of an intensity alarm. This pulse is given to the digital
output (Dig. Out). If you want to record the digital detector signal you need to use the RS232
serial connector.

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10.2INPUT-CONNECTORS
The RI2000 refractive index detector has three digital (TTL) inputs.
These can be used to control the system externally.
10.2.1 THE EXTERNAL START SIGNAL
Use the digital input connector (Dig.) to connect an external start signal (e. g. generated by
an autosampler or a manual injector) to the instrument.
10.2.2 THE EXTERNAL AUTOZERO SIGNAL
Use this input connector (AutoZero) to connect an external AutoZero signal to the
instrument.
10.2.3 THE EXTERNAL PURGE SIGNAL
Using this connector (Purge) you can use an external signal to activate the detector’s purge
mode.
■NOTE
All TTL signals handled by the RI2000 detector use a TTL level which is based on
instrument’s ground potential.
10.3THE RS232 PORT
The RS232 port can be used to acquire the detector’s signal using a personal computer as
well as to control the instrument using the computer. To communicate with the detector
using a computer you need to use a certain protocol which is explained in chapter 15.6 of
this manual.
10.4MASS SCREW
Use the mass screw to connect the shielding of the analog signal cable to the detector’s
chassis. This will result in a smoother detector signal.

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10.5OPTICAL ADJUST
The two black caps on the back side of the detector cover holes in the detector’s housing.
If needed the optical system of the detector can be adjusted using the hex-wrench which
came with the instrument. To adjust the mirror, remove these caps and turn the adjustment
screws carefully.
10.6DRAIN
In case of a leakage inside the housing mobile phase can leave the housing using the tube.
You might connect an additional waste tube to this exit.
10.7MAINS ADAPTOR
Use the power cable which was delivered with the detector to connect the instrument to the
power supply. Make surethat the correct voltage is selected before connecting to themains.
To high voltage will damage the instrument.
10.8FUSES
Next to the mains plug you can find the instrument’s fuses. The type of this fuse depends
on the voltage the instrument is operated.
220 V: 2 x 500 mA, slow
110 V: 2 x 1000 mA, slow
Inside the housing is an additional internal fuse (1 x 500 mA, slow).

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11 INSTALLATION OF THE RI2000
11.1CONNECTING THE DETECTOR TO THE CHROMATOGRAPHY SYSTEM
Connect the INLET on the front of the detectorto the capillary which comes from the column
of you chromatography system. To attach the column to the detector use a 1/16” stainless
steel capillary with 0.25 mm inner diameter.
Connect the 1/16” stainless steel capillary with 1 mm internal diameter to the PTFE tube
and the OUTLET port of the instrument. Use the screw connections to fix the capillaries to
the INLET and OUTLET port.
Place the free end of the PTFE tube in a bottle for solvent waste. The droplets leaving the
tube should run along the bottles wall and not fall down. The waste bottle and the refractive
index detector should be positioned at the same high level.
If you need a solvent mixture to perform your analytical separation it is recommended to
mix the different components manually before using the solvent.The use of a gradient pump
to generate a solvent mixture is not possible as the mixture generated by the gradient pump
is not consistant. Small changes in the solvent compositions will result in unstable detector
signals.
It is also recommended to degass the solvents before use with a refractive index detector
as this will result in a more stable detector signal.
■NOTE
Before dispatch of the instrument the flow cell was purged first with ethanol followed by air.
However there are still some rests of ethanol in the flow cell. For transportation or long time
storage of the instrument the procedure of purging with ethanol and air is recommended.
■NOTE
The flow cell is built of specialized optical glass which is sensitive to pressure. The
maximum pressure for the flow cell is 6 bar (0.6 MPa). If you want to use several detectors
is series make sure that the refractive detector is the last one in the rowto prevent damages
of the flow cell due to high pressure.

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11.2CONNECTION TO AN ANALOG DATA SYSTEM
Use a small screwdriver to connect the signal cable to one of the two pin connectors which
are delivered with your instrument. Connect the signal cable either to re integrator output
(Int. Out) or to the recorder output (Rec. Out) of the detector if you want to use an analog
integrator or recorder as well as an analog data system to collect data. Make sure that the
polarity (+/-) of the connection is correct.
■NOTE
The signal coming from the integrator output (Int. Out) is a voltage between -1 V and 1 V.
In case of a signal gain of 1 set in the detector parameters the signal at the recorder output
(Rec. Out) is the same.
If you need a very high sensitivity it is recommended to use the recorder output (Rec. Out)
as you can use the instrument’s internal signal amplifier which might amplify the detector
signal up to 16 times.
11.3CONNECTION TO A DIGITAL DATA SYSTEM (PC)
The RS232 port on the back side of the RI2000 refractive index detector can be used for
data acquisition as well as instrument control. Using the RS232 port for external instrument
control you might activate / deactivate the purge mode, send an external start / marker
signal and AutoZero signal.
To communicate with the RI2000 detector using the serial interface you will need a special
software package which utilizes a special communication protocol. Details of this protocol
you will find in chapter 15.6 of this manual.
There is a software package available which allows the data acquisition with the RI2000
detector. The data can be saved in user defined file formats for later data treatment using
chromatography software packages like PeakSimple or APEX.