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Analytik Jena SPECORD 200 Manual

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UV VIS Spectrophotometer
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SPECORD
200 / 205 / 210 / 250

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Summary of Contents for Analytik Jena SPECORD 200

  • Page 1 Accessories UV VIS Spectrophotometer ® SPECORD 200 / 205 / 210 / 250...
  • Page 2 + 49 (3641) 77-7407 Fax: + 49 (3641) 77-7449 e-mail: service@analytik-jena.de General information about Analytik Jena AG on the internet: http://www.analytik-jena.de Copyrights and Trademarks Microsoft, Windows 2000, Windows XP, Windows NT, MS Excel are registered trademarks of Microsoft Corp. 221:426.23 Publication No.:...

  • Page 3: Table Of Contents

    Adjustable holder for microcells, non-thermostatted (8.5 mm beam height)...23 Thermostatted cell holder..........25 Description and use..................25 Description .....................25 Using the thermostatted cell holder ..............25 8.3.1 Connection and installation in sample compartment ........25 ® User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 4 Design of Peltier-temperature-controlled cell holder, air-cooled .....57 ® 13.1.4 Installation of Peltier temperature-controlled cell holder in SPECORD ..58 13.1.5 Care .......................60 13.2 Peltier temperature-controlled cell holder with heat exchanger ......62 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 5 Mounting the sipper in the sample compartment..........99 14.3.3 Adjusting the flow cell...................100 14.4 Sample measurement ..................101 14.4.1 Settings on the PC ..................101 14.4.2 Performing a sample measurement .............102 14.5 Care and maintenance .................103 ® User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 6 Integrating Sphere............125 19.1 Description and use..................125 19.2 Design of integrating sphere ................126 19.3 Measurements with the integrating sphere...........127 19.4 Transmittance measurements ..............127 19.5 Reflectance measurements................129 19.6 Technical Data .....................133 Figures .................135 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 7: Introduction

    Chapters and illustrations are numbered consecutively. • Every illustration has its own caption. • Steps of operation are consecutively numbered. • Cross-references are marked by an arrow, e.g. → Section "Introduction" p. 1. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 8: Safety Notes

    Accessory-specific instructions are given in the chapter describing its use. Caution! Contamination! Never touch any optical mirrors of accessory units! Additionally, observe the operating instructions and safety notes of any supplied system components of other manufacturers (e.g. fluid thermostats User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 9: Care Of Accessories

    Two 9-pin connectors (3), (4) allow the connection of electrically driven accessories, such as the automatic temperature-controlled cell changer or the sipper system. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 10: Adjustment Of Zeroth Order

    Unscrew one of the carrying rails in the sample beam path (front pair) and remove the rod from the sample compartment. Screw one adapter (3) onto the carrying rail. Put the carrying rail onto the bottom, cone-shaped journal in the right-hand sample compartment wall. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 11 Fasten the knurled screw hand-tight so that the carrying rail cannot be moved. Repeat the above procedure for the second carrying rail. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 13: Universal Holder

    25 mm pathlength and a minimum diameter of ≥ 20 mm • Holder for round cells • Holder for semi-microcells and microcells Description Mounting plate for cell or solid sample holders Clamp lever Fig. 2-1 Universal holder User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 14: Using The Universal Holder

    You may also mount it inversely so that the plate (1) that accommodates the cell or solid sample holder is on the left-hand side. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 15: 100 Mm Cylindrical Cell (Absorption Tube)

    Slide holder (1) for cylindrical cells from top onto mounting plate (4) of the universal holder. Insert the 100mm cylindrical cell (5) flush right in holder (1) for cylindrical cells and slide the complete universal holder (2) assembly to the right-hand sample compartment wall. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 16: Care And Transportation Of Cylindrical Cell

    100 mm cylindrical cell (absorption tube) Care and transportation of cylindrical cell Store and carry the cylindrical cell only in the original packing. Clean the cylindrical cell after every use. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 17: Solid Sample Holder

    Insert sample (6) into holder so that it rests on mechanical stop (2). Push support block (5) towards the sample so that spring clips (3) safely hold the sample. Fasten knurled screw (4). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 19: Holder For Cylindrical Cells

    Put the cylindrical cell onto the support rods. If the thermostatted cell is being used, the thermostatting tubes must be threaded outside the sample compartment through the provided holes in the same way as with the thermostatted cell holder (→ see Section “Thermostatted cell holder”). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 21: Holder For Round Cells

    If this mark is missing, take several measurements and turn the cell between the measurements each to avoid pathlength errors in high-precision measurements. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 23: Holder For Semi-Microcells And Microcells

    Section "Universal holder" p. 11) and push it down as far as it will go. When you insert the semi-microcell, take care that the leaf spring definitely presses the cell against the left-hand wall. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 24: Adjustable Holder For Microcells, Non-Thermostatted, (8.5 Mm / 15 Mm Beam Height)

    (6) until the light appears centered on the cell aperture. Fine adjustment is done by taking an energy measurement: In the device driver (menu command: Measurement / Set Parameters), create a parameter record with e.g. the following parameters: User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 25: Adjustable Holder For Microcells, Non-Thermostatted (8.5 Mm Beam Height)

    Adjust the rider (3) using knurled screw (2) to suit the pathlength of the cell to be used. For this, unscrew rider (3) completely by means of knurled screw (2) and User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 26 Adjust the cell holder transversely to the beam by activating a transmission measurement program. Run repeated measurements and move the cell holder by turning knurled screw (4) until you obtain a maximum transmission value. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 27: Thermostatted Cell Holder

    If the tube is caught on these steps, try to loosen it by slightly turning it. When it becomes visible in the outer opening, you can bend it towards the opening e.g. by means of a pen. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 28: Inserting The Magnetic Stirrer

    Put the coil of the magnetic stirrer (4) into the square opening at the bottom of the thermostatted cell holder taking care that the flat cable (5) is flush with the bottom plate. Tighten knurled screws (8). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 29 (see above). 10. Put a stirring magnet into the cell and insert the cell in the holder. 11. Turn the speed control knob to adjust the stirring frequency. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 31: Adjustable Cell Holder, Thermostatted

    Screws for horizontal adjustment (2nd screw obscured) Top part of adjustable cell holder Lever Fig. 9-1 Adjustable thermostatted cell holder Sample feed Sample aspiration Beam aperture Fig. 9-2 HPLC cell User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 32: Inserting The Cell

    Repeat the adjustment procedure until the energy value of the sample beam I(M) has reached its maximum. Secure the optimum adjustment by retightening the four screws that fix the cell holder in position (5). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 33: 6-Cell Changer, Thermostatted

    In addition, a cell changer is available, which is designed for the accommodation of cells of 1, 2 and 5cm pathlength. However, this cell changer neither can be thermostatted nor equipped with magnetic stirrers. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 34: Design

    Thermostatted cell holder and driving unit Holder for magnetic coils of stirrer Magnetic coil under measuring position Flat cable Magnetic coil under the next position Fig. 10-2 Thermostatted cell holder with magnetic stirrer User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 35: Installation And Insertion In Sample Compartment

    Connect the connectors (Fig. 10-3 / 4) to the adapter (Fig. 10-3 / 5). Plug the adapter plug into the corresponding socket (Fig. 10-3 / 6) of the power supply (Fig. 10-3 / 7). Reattach the cell holder to its support on the driving unit. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 36: Connection To A Thermostat

    Depress the locking lever (4) and remove the male connector (2) from the quick-lock tube coupling. When you work with the device without cell changer, you may also leave the tubes with the quick-lock tube couplings in the tube ducts. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 37: Installation In Sample Compartment

    Replace the plastic foam stopper inserted in the recess of the sample compartment wall by the supplied plastic foam strips. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 38: Operation

    ® The cell changer is controlled via WinASPECT software. In the device driver dialog box (menu command: Measurement / Set Parameters), choose the 6-cell changer option on the Accessories tab. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 39: Fig. 10-6 Accessories Tab - Cell Changer

    Cell changer moves to the parking position with the cell block being centric above the base plate. In this position, the cell changer can be ® easily removed from and installed in the SPECORD as well as packed. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 40: Measurements With The 6-Cell Changer

    1, before the next cycle is executed for all samples. For the Slow time scan mode, observe the following notes regarding parameter selection: User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 41 Any activation of the Manual start check box will be disregarded. Instead, the measurement of the first sample begins after you confirmed the query "Start time scan?", whereas the measurement of all following samples will be started automatically. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 43: 8-Cell Changer

    Make sure to remove the red plastic foam pad from underneath the cell block before using the cell changer the first time. Replace this pad for any relocation of the cell changer. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 44: Design Of 8-Cell Changer

    Lay the connection tubes to the fluid thermostat tension-free to ensure freedom of motion of the cell block of the cell changer. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 45 Push the cell changer to the righ-hand sample compartment wall as far as it will go. Clamp it to the carrying rails by throwing the clamping lever over to the left. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 46: Operation Of The 8-Cell Changer

    The reference measurement is then integrated in the normal sample measurement process. Start manually If activated, a small dialog box appears: "Start cycle [OK]". The actual sample measurement is started only after you confirmed the User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 47: Measurements With The 8-Cell Changer

    Connect the cable of the cell changer in the rear reference beam path to the right- hand connector in the sample compartment. Connect the cable of the cell changer in the front sample beam path to the left-hand connector. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 48: Staggered Operation Of Two 8-Cell Changers For More Than 8 Samples

    In the presentation of the currently selected measurement parameters on the ® WinASPECT workplace, the assignment of cell positions is displayed according to your choice: User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 49: Synchronous Operation Of Two 8-Cell Changers

    To this end, load the samples in the front cell changer (in the sample beam path) while placing the corresponding references in the cell changer positioned in the reference beam path. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 50 Load the cell changer. Place the samples in the cell positions on the front cell changer and the references in the corresponding positions on the rear cell changer. Start the sample measurement. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 51: Cell Carousel

    Knurled screw Tray support with guiding slot Clamping lever Sample tray Stop bolt ® Cell holder Connection cable to SPECORD Handle Fig. 12-1 Cell carousel – Driving unit and sample tray User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 52: Installation In Sample Compartment

    Thread the connection cable underneath the rear carrying rails so that it does not project into the beam path. Insert the plug of the connection cable into the left connector in the sample compartment wall. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 53: Operation

    Accessories tab, choose the Carousel option. Set the operating parameters of the cell carousel analogously to the cell changer. Here, the maximum number of used cells is 15 (→ Section "6-cell changer, thermostatted, Operation", p.36). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 55: Peltier Temperature-Controlled Cell Holders/Cell Changers

    "Connection and operation of temperature control unit” p. 90. The heat exchanger used as counter cooler for cell holders/cell changers is described in Section "Connection and operation of the heat exchanger", p. 94 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 56: Peltier Temperature-Controlled Cell Holder, Air-Cooled

    The stirring speed is adjusted on the temperature control unit. Note The sample is optimally mixed up, if you use stirring magnets of 3 mm diameter and a length of 6 – 8 mm. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 57: Safety Notes

    • 73/23/EEC • 89/336/EEC It was delivered by Analytik Jena AG in perfect condition. To keep this condition and ensure safe operation, please observe the safety notes and the notes marked by symbols. Warning! Risk of electric shocks! Disconnect the power pug, before opening the instrument or removing any covers to avoid that components carrying line voltage or high tension become accessible.

  • Page 58: Technical Data Of Peltier Temperature-Controlled Cell Holder, Air-Cooled

    Data interface RS232 port Working temperature range +15°C...+35°C Transport and storage temperature range -40°C...+60°C Relative humidity up to 90% (at +30°C) Overview 13-2 Other technical data of Peltier temperature-controlled cell holder User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 59: Design Of Peltier-Temperature-Controlled Cell Holder, Air-Cooled

    Heat transfer device control device Heat-exchanger housing with Right guide rail stop intake slots Quartz window Clamping lever Lock screws Pressure plate Recess Fig. 13-2 Peltier temperature-controlled cell holder, air-cooled User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 60: Installation Of Peltier Temperature-Controlled Cell Holder In Specord

    (3). Take care that the cover of the sample compartment is not hindered by projecting plastic foam when closing the cover and make sure it closes light-tight. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 61: Fig. 13-4 Sample Compartment Cover With Cables Threaded Through

    Besides, this ensures the temperature constancy over the entire temperature range as specified. You need not lock the cap unless you use the cell-temperature sensor. To lock the cap, slightly twist it. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 62: Care

    On the bottom of the base plate (Fig. 13-5 / 1) there is a M4 Allen screw (Fig. 13-5 / 3) for draining the washing liquid. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 63: Fig. 13-5 Bottom Of Peltier Temperature-Controlled 1X Cell Holder

    These materials, too, are as far as possible corrosion-resistant. Caution! Ingress of solvents in the sensor! Avoid immersing the sensor completely in solvents, as they might enter the interior of the sensor. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 64: Peltier Temperature-Controlled Cell Holder With Heat Exchanger

    • 73/23/EEC • 89/336/EEC. It was delivered by Analytik Jena AG in perfect condition. To keep this condition and ensure safe operation, please observe the safety notes and the notes marked by symbols. Warning! Risk of electric shocks! Disconnect the power plug before opening the unit or removing any covers in order to avoid that components carrying line voltage or high tension become accessible.
  • Page 65 Particularly do not place any glasses or other vessels containing liquids on the device. When working with an aqueous system at temperatures below the freezing point there is the risk of cell damage by the expansion of ice. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 66: Technical Data Of Peltier Temperature-Controlled Cell Holder With Heat Exchanger

    IP 20 Data interface RS232 port Operating temperature range +15°C...+35°C Transport and storage temperature -40°C...+60°C range Relative humidity Up to 90% (at +30°C) Overview 13-4 Technical data of temperature control unit User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 67 Operating temperature range +15°C ... +35°C Transport and storage temperature range -40°C...+60°C Relative humidity up to 90% (at +30°C) Overview 13-5 Technical data of heat exchanger for PTC 600 / PTC 601 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 68: Design Of Peltier Temperature-Controlled Cell Holder With Heat Exchanger

    When it becomes visible in the outer opening, you can bend it towards the opening e.g. by means of a pen. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 69 13-6 / 9) are in line with the lock screws (Fig. 13-6 / 8). Pull the cover cap upward and carefully put the cell into the block. Finally, reattach the cover cap to the cell block. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 70: Fig. 13-7 Cell Temperature Measuring Sensor Pt100

    4 mm. This allows the cell sensor to be used in a certain range also for non-standard cells. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 71: Peltier Temperature-Controlled 6-Cell Changer

    Temperature control unit with status indicator for heat exchanger Heat exchanger Peltier temperature-controlled 6-cell changer ® Fig. 13-8 Peltier temperature-controlled 6-cell changer with SPECORD User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 72: Safety Notes

    The PTC 600 / PTC 601 Peltier temperature-controlled 6-cell changer was produced and tested in compliance with the following standards and regulations: • DIN EN 61010-1 (IEC 1010-1) • 73/23/EC • 89/336/EC User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 73: Technical Data Of Peltier Temperature-Controlled 6-Cell Changer

    Operating temperature range +15°C...+35°C Transport and storage temperature range -40°C ... +60°C Relative humidity up to 90% (at +30°C) Overview 13-7 Technical data of control device for PTC 600 / PTC 601 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 74 Pay attention to any different technical data on the type label! If the data given above are different from that on the type label, the data on the type label are valid. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 75: Design Of Peltier Temperature-Controlled 6-Cell Changer

    Stepper motor drive with lead screw Knurled screw for clamping the unit to the carrying rails Water tubes for connection to the heat exchanger Fig. 13-9 Design of Peltier temperature-controlled 6-cell changer User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 76: Installation Of The Peltier-Temperature-Controlled 6-Cell Changer

    Put the cell changer from top onto the front carrying rails of the sample compartment so that its guideways rest on the carrying rails. Then, push the cell changer to the right-hand sample compartment wall as far as it will go. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 77 On the Accessories tab of the measurement parameter window, activate the 6-cell changer (Peltier) option. If you intend to use standard cells (1cm x 1cm) or semi-microcells for the following analyses, perform the adjustment without any cells being inserted. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 78: Fig. 13-11 Cell Measuring Sensor For The Peltier Temperature-Controlled 6-Cell Changer

    0.1 – 0.2 degrees at increased settling time. However, the setting accuracy specified in Section "Technical data of Peltier temperature-controlled 8-cell changer", p.81 refers to the operation of the cell changer with heat exchanger. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 79: Settings In Winaspect ® Software

    Options for Peltier temperature-controlled 6-cell changer for SPECORD Option / button Description First sample Position of the first sample on the cell changer. Last sample Position of the last sample on the cell changer. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 80: Measurement Procedure

    Adjust the desired temperature on the temperature control unit (→ Section "Settings on temperature control unit", p. 91). The measurement procedure is analogous to that with the water-thermostatted 6- cell changer (→ Section " Measurements with the 6-cell changer", p.38). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 81: Peltier Temperature-Controlled 8-Cell Changer

    14 samples or to analyze every sample against a specific reference. The second cell changer needs a separate control unit. Countercooling is perfomed via a common heat exchanger. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 82: Safety Notes

    The control unit complies with the requirements of Protection Type IP 20. The Peltier temperature-controlled 8-cell changer was made and tested in compliance with the following standards and directives: • DIN EN 61010-1 (IEC 1010-1) • 73/23/EEC • 89/336/EEC User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 83: Technical Data Of Peltier Temperature-Controlled 8-Cell Changer

    Operating temperature range +15°C...+35°C Transport and storage temperature range -40°C...+60°C Relative humidity Up to 90% (at +30°C) Overview 13-10 Technical data of temperature control unit PTC 800 / PTC 801 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 84 Pay attention to any different technical data on the type label! If the data given above are different from that on the type label, the data on the type label are valid. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 85: Design Of Peltier Temperature-Controlled 8-Cell Changer

    Connector for connection to heat exchanger ® Connector for connection to SPECORD Water tubes for connection to heat exchanger S600 clamping lever Fig. 13-13 Design of Peltier temperature-controlled 8-cell changer User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 86: Installation Of Peltier Temperature-Controlled 8-Cell Changer

    Clamp it to the carrying rails by throwing the clamping lever to the left. Thread the connection cable to the SPECORD® to the back underneath the rear carrying rails and connect it to the left connector in the rear sample compartment wall. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 87 Lay the electrical connection cables as described above. Additionally fasten the supplied metal bracket above the recess in the sample compartment wall to avoid that the cables slip out of the recess. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 88 Start automatic adjustment by a click on the [Adjustment] button. Note The adjustment for two 8-cell changers is to be performed in the same way. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 89: Fig. 13-14 Cell Measuring Sensor For The Peltier Temperature-Controlled 8-Cell Changer

    This will result in a distortion of measurement results. For the beginning of condensation (dew-point temperature), the following relation applies: User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 90: Settings In Winaspect ® Software

    Before every measurement of a cell, a message box appears “Start cycle [OK]“. The actual sample measurement is started only after you confirmed this prompt. This option may be used, for instance, for kinetic User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 91: Measurement Procedure

    Adjust the desired temperature on the temperature control unit (→ Section "Settings on temperature control unit", p. 91). The measurement procedure is analogous to that with the water-thermostatted 6- cell changer (→ Section " Measurements with the 6-cell changer", p. 38). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 92: Connection And Operation Of Temperature Control Unit

    (Fig. 13-16 / 1) on the back panel of the temperature control unit. Connect the power cable to the power input connector (Fig. 13-16 / 3) and then to a power outlet. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 93: Settings On Temperature Control Unit

    The heat exchanger is connected to the control unit via the 6-pin connector, but has not been switched on. LED green The heat exchanger is connected to the control unit via the 6-pin connector and has been switched on. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 94: Fig.13-18

    O, Plastic 1x0.4 block temperature 2ml H O, Plastic 1x0.4 cell temperature 1000 Fig.13-18 Temperature distribution in cell block and in cell for different types of cells (measured on air-cooled, Peltier temperature-controlled cell holder) User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 95: Replacing Fuses On The Temperature Control Unit

    Replace the defective fuses considering the technical data of the cell holder or the cell changer you are using. Close the fuse holder again. Reconnect the power cable. ® Switch the SPECORD on again. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 96: Connection And Operation Of The Heat Exchanger

    13.6.2 Connecting the heat exchanger Connect the 7-pin connector of the cell holder / changer (with the appropriate connector (Fig.13-20 / 4) on the rear panel of the temperature-control unit. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 97: Replacing Fuses On The Heat Exchanger

    Replace the defective fuses considering the technical data of the cell holder or the cell changer you are using. Close the fuse holder again. Reconnect the power cable. ® Switch the SPECORD on again. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 99: Cassette Sipper

    Fig. 14-1 Design of cassette sipper The cassette sipper consists of: • Adjustable holder for flow cells of 1, 2, and 5 cm pathlength • Peristaltic pump • Tube set. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 100: Mounting The Cassette Sipper

    Insert the cell in the cell holder with the outlet connector facing the pump. Fasten the tube cassette to the pump rollers (Fig. 14-1). Press the pump tube to the rollers with the eccentric so that it is fully squeezed. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 101: Mounting The Sipper In The Sample Compartment

    To position the flow cell as close to the detector as possible, push the sipper system to the right against the sample compartment wall. Clamp the sample holder by means of the clamping lever. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 102: Adjusting The Flow Cell

    Successively turn the vertical and horizontal adjusting screws and, after every adjustment, measure the energy with the sample compartment cover closed. Repeat the procedure until the energy of the sample beam I(M) has reached its maximum value. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 103: Sample Measurement

    Click on the Pump ON button if you want to check the aspiration process or determine the optimum pump time. The label of this button changes depending on the switching state of the pump. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 104: Performing A Sample Measurement

    When the measurement process is finished, a message window appears prompting you to prepare the wash solution. Bring the wash solution to the aspirating tube. Start the wash process with [OK]. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 105: Care And Maintenance

    When you finished working with the sipper, detach the tube cassette from the pump rollers thus slackening the pump tube. In this way, the elasticity of the pump tube is maintained longer. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 107: Apg 53/100 Xyz Autosampler

    Do not fold the sample tube! Take care that the sample tube is not folded! Folds in the tube will hinder sample flow. Do not reel up the sample tube in narrow bends! User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 108: Design And Installation Of The Apg 53/100

    Knurled screw for fixing the aspirating tube Tube holder Stirring bracket carrying the movable magnetic stirrer underneath the current sample cup Rinse vessel Guiding arm Fig. 15-1 APG 53 (front view) User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 109: Fig. 15-2 Connections Of Apg53 (Rear Panel)

    Tighten the knurled screw (10). If mounted properly, the middle of the stirrer plate is exactly underneath the tube holder. The bracket points to the back and projects under the basic device. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 110: Connecting The Xyz Autosampler To The Specord

    Shift the MFA tube within the black guiding tube so that the following tube length juts out from the guiding tube: APG 53 80 mm APG 100 100 mm User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 111 Switch on autosampler (18, Fig. 15-2). ® Switch on PC and SPECORD ® ® Start WinASPECT software and initialize the SPECORD Activate the device driver (measurement parameter dialog box). User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 112: Sample Measurement

    After a click on [Reference], a small dialog box appears showing the list of samples. Mark the tray position(s) accommodating the reference(s). The selected positions appear beside the [Reference] button. Maximum number of selectable references: 10 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 113: Finding The Appropriate Pump Time

    That way, the cell can be rinsed with the sample before the measurement and carry-over errors be minimized. Enter the found optimum pump time in the measurement parameters of the XYZ sampler. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 115: Fiber Coupling For Measuring Probes

    (4). A second optical fiber (3) transmits the light attenuated by the sample in the measuring probe back to the adapter (1). The adapter couples the attenuated light into the sample beam. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 116: Design And Function Of The Fiber Coupling With Sma Connectors

    If you use optical fibers with SMA connectors, first connect the fibers with the measuring device to be used for the analysis. To do this, proceed as described in Section “Adjustable holder for microcells, non- thermostatted (8.5 mm beam height)” p. 23. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 117: Absolute Reflectance Attachment

    Sample locating plate Fixed mirrors Carrier for swivel mirror Clamping lever Swivel mirror Stop screw to sample compartment wall Stop screw for "W" beam configuration Sample holder Fig. 17-1 Absolute reflectance attachment User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 118: Installation In Sample Compartment

    Withdraw sample holder from locating plate (10) Put sample to locating plate and let sample holder return until it touches the sample. The measurement is taken at a reflecting angle of 7°. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 119: Adjustment

    When the reference measurement is finished, turn the unit to set it for "W" beam configuration. Withdraw sample holder (10) from sample locating plate (2), insert the sample (1) and let the sample holder return to the sample. Take the sample measurement. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 120: Care And Maintenance

    Then, wipe with a new cotton swab soaked with distilled water only. Finally, dab metal mounts dry. • Carry and store the absolute reflectance attachment only in a closed box. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 121: Variable Angle Reflectance Attachment

    Measuring aperture Beam exit Fig. 18-1 Reflectance attachment with large sample table The accessory has a base plate (1) that accommodates imaging and reflecting optics as well as the sample table. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 122: Fig. 18-2 Mirror And Small Tabletop

    Point support to protect the sample surface from scratches Fig. 18-2 Mirror and small tabletop Quartz lens Reflecting mirror Plane mirror Sample Fig. 18-3 Optical path in reflectance attachment (front view) User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 123: Installation In Sample Compartment

    – Sample measured in W configuration Sample Sample - Reference measurement in V Reference Reference configuration – Intensity after reflection at the reference mirror ference reference beam – Intensity in reference beam path Reference beam User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 124: Calculating Pathlength And Refractive Index

    For that, in ® WinASPECT software, use the Peaklist function of the Data Handling menu. Example: Measuring curve Example of interferences at an angle of reflection Θ = 60° Fig. 18-4 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 125: Care And Maintenance

    165 mm x 115 mm x 135 mm Size of large tabletop 115 mm x 80 mm Size of small tabletop 70 mm x 80 mm Weight ca. 2 kg User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 127: Integrating Sphere

    (grain size 220 – 240). Subsequently wash the surfaces with distilled water and then dry them with compressed air. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 128: Design Of Integrating Sphere

    It is placed with its locating surfaces (14), (15) or (16) onto the carrying rails in the ® sample compartment of the SPECORD User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 129: Measurements With The Integrating Sphere

    Fig. 19-2 illustrates the optical path in transmittance measurements of a scattering sample. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 130: Fig. 19-2 Optical Path In Transmittance Measurements

    (Fig. 19-1 / 18) in aperture (Fig. 19-1 / 11). Screw in locating pin (Fig. 19-1 / 12) to ensure correct position of the insert. Adjust stop (Fig. 19-1 / 4) to the desired beam transmission height. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 131: Reflectance Measurements

    The sphere captures the radiation reflected by the sample and sends it diffusely to the detector of the ® SPECORD User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 132: Fig. 19-3 Optical Path In Reflectance Measurements

    (Fig. 19-1 / 17) is well visible. For the measurement of powder samples, insert the sphere in such a way that the samples are always at the bottom of the sphere. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 133: Fig. 19-4 Integrating Sphere With Sample-Loading Fixture

    Place the sphere onto the support (Fig. 19-4 / 4). Turn knurled screw (Fig. 19-4 / 6) to move the thrusting disk (Fig. 19-4 / 5) towards the sphere body. Fasten the knurled screw only as much as is necessary to hold the sphere body reliably. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 134 Quantitative Analysis. Then, as you are used to do from concentration determination in Quantitative Analysis, measure the unknown sample based on the found calibration curve. User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 135: Technical Data

    (L x W x H): Samples for diffuse reflectance Diameter up to 50 mm Depth up to 20 mm Sample holder for powder samples Diameter 16 mm Depth 5 mm User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

  • Page 137: Figures

    Installation of the PTC 100 in the sample compartment ......58 Fig. 13-4 Sample compartment cover with cables threaded through ......59 Fig. 13-5 Bottom of Peltier temperature-controlled 1x cell holder ......61 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...
  • Page 138 Fig. 18-4 Fig. 19-1 Integrating sphere with accessory items ..........126 Fig. 19-2 Optical path in transmittance measurements...........128 Fig. 19-3 Optical path in reflectance measurements..........130 Fig. 19-4 Integrating sphere with sample-loading fixture.........131 User’s Manual SPECORD 200/205/210/250 – Accessories 07/2005 Analytik Jena AG...

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