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Schambeck RI 2012, Руководство по эксплуатации

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Schambeck SFD GmbH 

 

Refractive Index Detector RI2012 

 

 

RI2012 V1.0 06-2013.EN / 28.10.2013 

19 

http://www.schambeck-sfd.com 

 

12 P

RINCIPLE OF 

D

ETECTION

 

The RI2012 refractive index detector acts as a differential refractometer which measures the 

deflection  of  a  light  beam  as  a  result  of  different  refractive  indices  of  solutions  in  the 

reference and the sample chamber of the flow cell. 

The beam of a tungsten lamp passes a convex lens and two slip apertures (called slit 1 and 

slit 2) before reaching a second convex lens. After this the light passes the flow cell which is 

diagonally separated into two chambers (sample and reference chamber). Behind the flow 

cell a mirror is placed which reflects the beam through the flow cell, the second convex lens 

and the second slit aperture (slit 2) toward a light sensor. 

The light sensor is placed under the light source and consists of two photo diodes. The both 

diodes  generate a  current  which  is  proportional  to  the  light 

intensity reaching the sensor’s 

surface. 

 

 

12.1  T

HE 

O

PTICAL 

S

YSTEM OF THE 

RI2012 

 

 

 

Содержание RI 2012

Страница 1: ...RI 2012 Schambeck SFD GmbH Drieschweg 13A D 53604 Bad Honnef Germany Telephone 49 0 2224 9239 0 Telefax 49 0 2224 9239 20 http www schambeck sfd com...

Страница 2: ...Version 1 01 Printed 28 10 2013 File RI2012 V1 0 english 10 2013 doc Last modified Makowski...

Страница 3: ...MENU BUTTON 12 9 8 THE ENTER BUTTON 13 9 9 THE IN PORT 13 9 10 THE OUT PORT 13 10 THE BACK SIDE OF THE RI2012 14 10 1 OUTPUT CONNECTORS 14 10 1 1 THE INTEGRATOR SIGNAL OUTPUT 14 10 1 2 THE RECORDER S...

Страница 4: ...THE SERVICE MODE 35 15 1 FIRMWARE INFORMATION 36 15 2 VIEWFINE MODE 37 15 3 ADJUSTING DIGITAL ANALOG CONVERTERS 39 15 4 CALIBRATING THE RI2012 40 15 4 1 HOW TO CALIBRATE 41 15 5 SERVMODE OVERVIEW 44 1...

Страница 5: ...d com 1 CONTACT ADDRESS In case of problems with your RI2012 refractive index detector please contact your local distributor or Schambeck SFD GmbH Schambeck SFD GmbH Drieschweg 13 A D 53604 Bad Honnef...

Страница 6: ...index detector In case of any question please do not hesitate to contact you local distributor or Schambeck SFD GmbH directly 3 ELECTRICAL WARNINGS Before opening the housing of the instrument make su...

Страница 7: ...at 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 det...

Страница 8: ...ch 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...

Страница 9: ...tal output 3 nRIU 3 V Drift 1 RIU h 1mV h Integrator output 1 2 V fix Recorder output 1 2 V adjustable Recorder range 8 steps selectable in the region from 1 8 to 16 1 Recorder offset Selectable 0 mV...

Страница 10: ...13 EN 28 10 2013 8 http www schambeck sfd com 6 PHYSICAL SPECIFICATIONS Dimensions 300 mm 175 mm 440 mm W H D Weight 9 6 kg Voltages Mains adaptor with voltage selector 100 120 V 220 240 V Frequency 5...

Страница 11: ...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 over...

Страница 12: ...ry 0 25 mm inner diameter 1 59 mm outer diameter for sample entry 1 EA Stainless steel capillary 1 00 mm inner diameter 1 59 mm outer diameter for sample exit 1 EA PTFE tube 1 59 mm inner diameter 2 8...

Страница 13: ...splay 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...

Страница 14: ...ignal 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...

Страница 15: ...for the mobile phase coming from the column Connect the capillary coming from the column to this port using screw connectors 9 10 THE OUT PORT This is the exit of the mobile phase Connect you waste bo...

Страница 16: ...ce 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 recorde...

Страница 17: ...this connector Purge you can use an external signal to activate the detector s purge mode NOTE All TTL signals handled by the RI2012 detector use a TTL level which is based on instrument s ground pot...

Страница 18: ...t screws for the mirror Keep in mind that you might have to turn the other screw Anyway you should turn the screws not more that 1 5 1 8 turns Adjust the screws until the optical balance reaches a val...

Страница 19: ...ent 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 po...

Страница 20: ...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 3 CONNECTION...

Страница 21: ...convex lens and two slip apertures called slit 1 and slit 2 before reaching a second convex lens After this the light passes the flow cell which is diagonally separated into two chambers sample and re...

Страница 22: ...heat exchanger to ensure that the measurement is performed at constant temperatures as the refractive index is highly dependent on the temperature The temperature for the optical bench can be selected...

Страница 23: ...ssing the heat exchanger again the liquid reaches the T connector and after this it reaches the flow cell Now the reference chamber is flushed by mobile phase Leaving the flow cell the liquid is guide...

Страница 24: ...Schambeck SFD GmbH Refractive Index Detector RI2012 RI2012 V1 0 06 2013 EN 28 10 2013 22 http www schambeck sfd com 14 OPERATING THE RI2012 DETECTOR 14 1 OVERVIEW FIRMWARE VERSION 5 2...

Страница 25: ...o is shown in the display the LEDs will light up for a short time and an acoustical signal will occur The initialization procedure will be finished after approx six seconds and the detector will switc...

Страница 26: ...bench in C Line 2 shows the optical balance between the two photo diodes of the light sensor in which corresponds with the relative position of the light beam on the surface of the light sensor Line...

Страница 27: ...settings ComRS232 Settings for serial RS232 port Another function of the status line is the input of new parameter settings by the user The symbol represents the four ARROW keys stands for the ENTER...

Страница 28: ...eat up when operated As a result of this the temperature can be controlled in a range from 35 C up to 55 C only To change the temperature setpoint press the ArrowUp to switch to higher temperatures or...

Страница 29: ...ove 64 C In this case the error message will be shown in the display and a periodic acoustic signal occurs The acoustic signal will stop when the temperature reaches the range between 9 C and 64 C NOT...

Страница 30: ...r different modes for signal smoothing RAW No signal smoothing FAST Signal smoothing by calculating the average in a time interval of 0 4 seconds MEDIUM Signal smoothing by calculating the average in...

Страница 31: ...llows to amplify or attenuate the detector signal at the recorder output RecOut If the amplification mode is set to 1 1 the signal at the recorder output Rec Out corredsponds to the signal at the inte...

Страница 32: ...ttons ArrowUp and ArrowDown you can either add a static voltage to each data point recorded by the detector detector offset or define a maximum voltage for the detector signal detector extent 14 7 1 R...

Страница 33: ...TENT To adjust the recorder extent press the ArrowUp button until the following status line is displayed Using the ArrowUp button you can switch to higher maximum voltages the ArrowDown button leads t...

Страница 34: ...rder output Is the parameter UseMarker set to NONE no marker signal can be sent to the recorder Pressing one of the buttons ArrowUp or ArrowDown changes the setting to ARROW To accept this setting pre...

Страница 35: ...32 you may adjust the parameters for the serial data interface If the mode is set to LOCK no detector is sent to the RS232 port Use this setting only in that case you want to record your data using an...

Страница 36: ...Enter Enter Enter N o r m M o d e In this mode the user can adjust several parameters fort he operation of the RI2012 refractiv index detector The Norm Mode is used to Display temperature C optical b...

Страница 37: ...ds The display will change from normal measuring mode NormMode to service mode ServMode The numerical values for temperature optical balance and the current detector signal are now displayed with thre...

Страница 38: ...h as the firmware version number or the instrument s serial number press the MENU button in service mode until the menu SwHwInfo is shown in the status line Then press the ENTER button The display wil...

Страница 39: ...this mode press the MENU button until the sub menu ViewFine is shown in the status line Now press the ENTER button and the display will change to the following information The values in line two repr...

Страница 40: ...e part of the light sensor Smpl Sample voltage Corresponding to the light intensity on the sample side of the light sensor Rfrn Reference voltage Corresponding to the light intensity on the reference...

Страница 41: ...unction allows the user to apply a defined signal to the recorder output and the integrator output NOTE Make sure that the signal amplification for the recorder output is set to 1 1 before using this...

Страница 42: ...cations of the optical system only Under normal operation conditions a re calibration of the RI2012 is not needed To calibrate the signal response of the instrument you need a solution of exactly 106...

Страница 43: ...ion will be shown in the display DifW Difference with water SumW Summ with water Dift Difference with test solution SumW Summ with test solution By pressing the ENTER button you can see the current SP...

Страница 44: ...owing view The signal is recorded and checked In the display line two the difference voltage Diff 0100 in this example and the sum voltage Summ 5030 in this example is shown If the signal is stable th...

Страница 45: ...button to finish the calibration process The new calibration factor is shown in the upper right corner of the display The four measured and calculated voltages are shown in the display according to th...

Страница 46: ...eatures on service mode More detailed display 3 decimal places of temperature C optical balance and detector signal mV System information such as firmware version and serial number of the instrument D...

Страница 47: ...ctions LOW 0 4 Hz serial port open 0 4 data point sec sent 1 Hz serial port open 1 data point second sent 2 Hz serial port open 2 data point second sent 5 Hz serial port open 5 data point second sent...

Страница 48: ...px 2 Disconnect the RI2012 from Computer 3 Install the CP210x VCP Drivers for RI2012 USB interface Follow the installation instructions on the screen 4 Reboot Computer 5 Connect RI2012 with A B USB ca...

Страница 49: ...of the detector Press the buttons ArrowLeft and ArrowRight at the same time for approx three seconds The display will switch into service mode Press the MENU button until the menu SwHwInfo is shown in...

Страница 50: ...OF THE TEMPERATURE SENSOR There are two possible error messages indicating problems with the temperature sensor A more detailed description of the temperature control of the RI2012 can be found in cha...

Страница 51: ...this message noAD shows up the analog digital converter did not connect to the micro controller Switch of the instrument wait for ten seconds and try to start again If the problem remains contact the...

Страница 52: ...ero and Polarity are only active if there is a detector signal Is the message SIGNAL too low displayed the voltage USumm is below 1 7 V The reason is low light intensity reaching the light sensor To r...

Страница 53: ...he following table xx 1H sample voltage beyond 5 V xx 2H reference voltage beyond 5 V xx 1L sample voltage below 0 V xx 2L reference voltage below 0 V The sample voltage corresponds to the light inten...

Страница 54: ...is switched on If the error message RC is shown in the display the controller was not able to load the internal configuration during the initialization In this case for example the calibration factor...

Страница 55: ...irror During the procedure you can follow the changes by observing the change of the detector signal or more detailed by observing the difference and sum voltage For the calculation of the different v...

Страница 56: ...of the opened hole at the back side of optical system NOTE There are two adjustment screws for the mirror Keep in mind that you might have to turn the other screw Anyway you should turn the screws not...

Страница 57: ...do the following steps Switch off the instrument Unplug the mains cable to prevent electrical shock when opening the housing NOTE Some operations during the adjustment have to be done when the instrum...

Страница 58: ...13 EN 28 10 2013 56 http www schambeck sfd com Loosen the holding screw of the light source and remove the lamp Loosen the screw connector of the lamp s power supply at the pre amplifier board labelle...

Страница 59: ...ltage at the test points on the circuit board The label of this test point points are Lampe ULmp and GND The lamp voltage should be 3 7 0 5 V If needed you can adjust this voltage by turning the poten...

Страница 60: ...sfd com Make sure that only 2 3 of the slit are illuminated by the light source This is illustrated in the following figure NOTE The projected picture at the light sensor should be a sharp one The fu...

Страница 61: ...optical balance should be 0 20 0 To ensure a stable temperature the instrument should be switched on for several hours before performing this test Press the PURGE button Make sure the purge mode is a...

Страница 62: ...s the difference voltage in mV and corresponds to the difference of intensity reaching the sample side and the reference side of the light sensor Summ represents the sum voltage in mV and corresponds...

Страница 63: ...ower cables of the light source to make sure that they are connected properly If needed check the light source see chapter 16 4 NOTE Both chambers of the flow cell are filled with the same solvent wit...

Страница 64: ...ected before opening the housing of the instrument Remove the stainless steel capillaries from the valve body NOTE Remind the position of the capillaries for proper re connection Loosen the control ca...

Страница 65: ...g the flow cell Drop of the sum voltage below 4500 mV Make sure that your sample chambers are washed and filled with distilled water without bubbles before checking the sum voltage Noisy baseline may...

Страница 66: ...reason it is not recommended to store the detector for a longer time with aqueous solvents inside For long time storage it is recommended to purge the flow cell with ethanol followed by air If possib...

Страница 67: ...radiated of electronic compounds In the interval from 35 C up to 55 C the temperature can be selected in 1 C steps The temperature difference of 6 C has to be considered If the heating is activated a...

Страница 68: ...e test points on the board The figure on page Fehler Textmarke nicht definiert shows the board used in instruments if the 0312xxx series The figure on page Fehler Textmarke nicht definiert shows the b...

Страница 69: ...flow cell seals 4 pcs for RI2012 Nessesary for all typs of flow cells RI2012 001 Flow cell analytical version RI2012 RI2012 003 Flow cell holder analytical version RI2012 RI2012 030 Flow cell micro v...

Страница 70: ...und Laborger te 89 336 EWG Elektromagnetische Vertr glichkeit EMV DIN EN 50081 Fachgrundnorm St raussendung EN 55022 Messung der Funkst rspannung von 150 kHz bis 30 MHz EN 55022 Messung der Funkst rfe...

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