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- Frank`s Hospital Workshop

1. A heat exchanger is used for the counter cooling of the Peltier elements The cell sensor is specially designed for standard cells with round PTFE stopper This sensor can be left in the cell when taking the optical measurement Caution Risk of getting faulty results When using other types of cell the measuring sensor may project into the the sample beam and thus distort the results of measurement The standard equipment of the cell holder includes a magnetic stirrer in order to obtain fast and homogeneous temperature adjustment in the cell The stirring speed can be adjusted on the temperature control unit Note Samples are optimally mixed when using stirring magnets of 3mm diameter and 6 to 8 mm length Safety notes The Peltier temperature controlled cell holder has been made and tested in compliance with the following standards and directives e DIN EN 61010 1 IEC 1010 1 e 73 23 EEC e 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 Only connect the power cable to a power outlet having an earth conductor to ensure operation of the unit according to Protection Class I earth conductor conn
2. 11 5 2 Synchronous operation of two 8 cell changers In synchronous operation of the two cell changers every sample is analyzed against a sample specific reference Hence you can simultaneously analyze a maximum of eight samples with their corresponding references 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 47 Analytik Jena AG 8 cell changer Measurement parameters for synchronous operation The following measurement parameters must be selected specifically for the synchronous operating mode General tab Correction Select the Reference option Accessories tab 2 x 8 cell changer selected 1 sample reference To be deactivated To be activated Cell changer First sample a Nos 4 Pos 1 Last sample No 8 Fos 1st sample Reference i R Synchron Manual Start T Adjustment Slow time scan Parking Fig 11 5 Software settings for the combination of two 8 cell changers in synchronous mode Taking measurements in synchrounous operation 1 Take the reference measurement with blank cell changers 2 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 3 Start the sample measurement 48 Users Manua
3. Cassette sipper 14 5 Care and maintenance Maintenance Maintenance on the cassette sipper is restricted to replacing the pump tubes Section Mounting the tube set p 98 Pump tubes of other materials or with different inside diameters can be ordered from our Service Department Care Observe the following advice on device care e Avoid any contamination on the sample holder Wipe off spilt samples or reagents instantly with an absorbent cloth or tissue Remove sticking dirt with a soft cloth moistened with a commercial detergent e When you finish using the sipper fill the flow cell with distilled water When the cell dries out sample residues may remain stuck to the flow cell e 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 103 Analytik Jena AG APG 53 100 XYZ Autosampler 15 APG 53 100 XYZ Autosampler 15 1 Intended use The APG 53 100 is an XYZ autosampler Used in combination with a sipper it serves to transfer the sample to the flow cell in the spectrophotometer The autosampler is controlled by the PC The APG is supplied with a sample rack for 53 sample cups APG 53 and equipped with a magnetic stirrer In addition an upgrade kit is available for a sample rack with 100 sample cups without stirrer AP
4. Measurements with the 6 cell changer p 38 11 5 Use of two 8 cell changers You can also use two 8 cell changers in combination This way it is possible to analyze every sample against a specific reference synchronous operation or to increase the number of samples analyzed within a measurement series Staggered operation To this end install the second cell changer analogously to the first one clamping it to the carrying rails in bottom position in the reference beam path Section Installation of 8 cell changer p 42 Align the two 8 cell changers in the same way as a standard cell changer If the cell changers shall be temperature controlled by an external thermostat connect the two cell changers with each other by a short piece of tube Lay a connection tube each from every cell changer to the thermostat Caution Ensure correct connections in sample compartment 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 45 Analytik Jena AG 8 cell changer The software settings for the combined use of two 8 cell changers are to be selected on the Accessories tab after having activated the 2 x 8 Cell changer option The major functions available are the same as those for a single 8
5. Peltier temperature controlled 6 cell changer Technical data of heat exchanger WC 600 WC 601 72 Weight without coolant 3 2 kg Dimensions W x H x D 225 x 175 x 200 mm Line voltage 220 240 V Line frequency 50 Hz Power consumption 50 VA Line fuses for WC600 2x T 0 5 A H 250V Type 19181 Wickmann Line fuses for WC600 2x T 1 6 A H 250V Type 19181 Wickmann EMC jamming and noise immunity as per DIN EN 61326 and 61326 A1 The device can be installed and operated in all environments Fire resistance of the case of the heat HB 1 6 exchanger according to UL94 Protection Type IP 20 Coolant Approximately 0 4 distilled water with an addition of 4 ml isopropanol Maximum delivery head 1 2m Operating temperature range 157 35 C Transport and storage temperature range 40 C 60 C Relative humidity up to 90 at 30 C Overview 13 8 Technical data of heat exchanger for PTC 600 PTC 601 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 13 3 4 Design of Peltier temperature controlled 6 cell changer 1 2 3 4 Cell block with insulation Block sensor Connector for
6. c ceee 84 13 4 5 Settings in WINASPECT software c cccscsscecesssesesesesceveceserereeveseeerereeveveenen 88 13 4 6 Measurement procedure ccccccseseeccecceeeececccaueeceeceauececseauueeeeessaeeeeessaageeess 89 13 5 Connection and operation of temperature Control UNIt cccceeeeeeeeeeeeeeeeees 90 13 5 1 Connecting the temperature control unit cece eeeeeccceceeeeceeeeeeeeeeeeeeeeeeeeeas 90 13 5 2 Settings on temperature control UNIt eee ecccccecceeseeeeeeeeeseeeeeeeeeeeeesseaeeeees 91 13 5 3 Replacing fuses on the temperature Control unit cccceceeeeeseeeeeeeeeeeeeeees 93 13 6 Connection and operation of the heat Exchange ccccccecsseeeeeeeeeeeeeeeeees 94 13 6 1 Prepanng Ne Coolant arreen es Ba ah ak Se a ee al eat cela 94 13 6 2 Connecting the heat exchange h enire E 94 13 6 3 Replacing fuses on the heat exchanger csscccccseeeecceeeeeceeeeeeseueeeseeneeeens 95 14 Cassete SIPpera nenne see ursenseenecencesseeecnte 97 14 1 Mende US Enersen a 97 14 2 Design Of cassette SiIPDET nadira a a a a sdaed ede 97 14 3 Mounting the cassette sipper cccecccceseeecceeeeecceeeeeceaeseeceaseesseeeeeseneeessees 98 14 3 1 Mounting the tube SCL aacctickccc ciate Rice lke Raed oie etn tecaa 98 14 3 2 Mounting the sipper in the sample CompartMent eeeeeeeectteeeeeeeeeeeeaes 99 14 3 3 Adjusting the flow Cell z 32cec2enssaidest acta taccecdede bere dens acl Wecdeeccet
7. 5 C 65 C PTC 801 with heat exchanger WC 601 20 C 105 Setting accuracy 0 1 degree Reading accuracy 0 1 degree Regulating accuracy 0 1 degree Temperatures below room temperature may result in steaming up of cells Overview 13 9 Technical data of Peltier temperature controlled 8 cell changer Technical data of temperature control unit Dimensions W x H x T Line voltage Line frequency Power consumption Line fuses EMC jamming and noise immunity as per DIN EN 61326 and 61326 A1 Fire resistance of the case of the control unit according to UL94 Protection Type Data interface Operating temperature range Transport and storage temperature range Relative humidity Weight 2 5 kg 225 x 130 x 200 mm 100 240 V 15 10 50 60 Hz 150 VA 2 x T 2 5 A H 250V Type 19181 Wickmann The device can be installed and operated in all environments HB 1 6 IP 20 RS232 port 15 C 35 C 40 C 60 C 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 81 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 82 Technical data of heat exchanger Weight without coolant Dimensions W x H x D Line voltage Line frequency Power consumption Line fuses for WC 60
8. Adjustment of the Peltier temperature controlled 8 cell changer The cell changer can be adjusted computer controlled to optimally position the cells in the beam Adjustment is necessary 4 e Atthe first use of the cell changer e After wavelength calibration e After relocation of the SPECORD e When working with microcells Install the empty cell changer in the sample compartment On the Accessories tab of the measurement parameter window activate the 8 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 If you intend to use microcells in the analyses insert a microcell filled with water in every of the six positions Start automatic adjustment by a click on the Adjustment button EF 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer Monitoring the cell internal temperature rE 1 Cell sensor 2 Connector for cell sensor Fig 13 14 Cell measuring sensor for the Peltier temperature controlled 8 cell changer 1 Close a standard cell with round stopper with the supplied cell measuring sensor Fig 13 14 1 in place of the standard stopper 2 Put the cell onto an
9. 1 Install the empty cell changer in the sample compartment 2 Onthe Accessories tab activate the 6cell changer option 3 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 If you intend to use microcells in the analyses insert a microcell filled with water in every of the eight cell positions 4 Start automatic adjustment by a click on the Adjustment button 11 4 Operation of the 8 cell changer 11 4 1 Software settings The cell changer is controlled by WinASPECT software On the Accessories tab of the measurement parameter window choose the 8 cell changer option Cell changer First sample b No 1 Fos 1 Last sample Ho g Pos 1 1st sample Reference E Adjustment Manual Start L J Slow time scan I Parking Fig 11 2 8 Cell changer options for the SPECORD Parameter Description Button First sample Position of the first sample on the cell changer Last sample Position of the last sample on the cell changer 1st sample To be activated if the first place on the cell changer holds the reference reference In this case it is not necessary to take a separate reference measurement 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
10. 13 Stirrer bracket carrying the movable magnetic stirrer underneath the current sample cup 16 Connector for connection to SPECORD 17 Diode connector for connection of magnetic stirrer 18 Power switch assembly 19 230V 115V line voltage selector 20 Appliance mains input connector Fig 15 2 Connections of APG53 rear panel Installation of XYZ autosampler When installing the autosampler additionally observe the description provided by the manufacturer 1 2 Put the XYZ autosampler on its rear side Remove the red transport lock To this end unscrew the two screws located on the underside of the device Further installation procedure for the APG 53 model 3 Push the four feet into the foot sockets and fasten the feet with knurled screws 4 Put the XYZ autosampler upright on the table and check its stability Readjust the feet if necessary 4 Slide the stirrer bracket onto the underside of the Z dome into the grooves Align the bracket so that it is centered 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 107 Analytik Jena AG APG 53 100 XYZ Autosampler 5 Put the base covering from the front onto the basic device and fasten it by means of the four bolts 2 The stirrer bracket is now under the base covering
11. Changing the position of the carrying rails p 8 3 Place the cell changer onto the relocated carrying rails with its clamping lever facing the back Push the cell changer to the right hand sample compartment wall as far as it will go Clamp it to the carrying rails by throwing the clamping lever to the left 4 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 5 Put the electrical cables 3 into the recess in the rear sample compartment wall 4 and close the recess again using the plastic foam strips Fix the plastic foam strips by attaching the supplied metal bracket Make sure that the recess is closed light tight SPECORD with recess underneath the sample compartment cover 6 Thread the cables through underneath the sample compartment cover and put the cable into the recess so that they are not squeezed when you close the cover SPECORD without recess underneath the sample compartment cover 6 Remove the knurled screws from the cover prop Fold the cover backward Put the connecting plug of the electrical cables 3 through the slit between the sample compartment cover and the SPECORD basic device Screw on the cov
12. Slide the thermostatted cell holder with its guide 6 from top onto the mount for cell holders Fig 1 1 10 or the mounting plate of the universal holder Inserting the magnetic stirrer Caution Incorrect line voltage may damage the unit Make sure the operating voltage of the power supply unit 7 agrees with the available line voltage 1 Knurled screws 5 Flat cable for connector 2 Bottom plate 6 Connector 3 Metal block 7 Power supply with speed control 4 Coil of magnetic stirrer 8 Knurled screws Fig 8 2 Inserting the magnetic stirrer coil Attach the magnetic stirrer before you insert the cell holder in the sample compartment 1 Loosen knurled screws 1 on the underside of the thermostatted cell holder and remove bottom plate 2 Remove metal block 3 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 Thermostatted cell holder 5 Without twisting the flat cable thread it under the rear carrying rails and through the stopper in the rear wall of the sample compartment Fig 1 1 5 6 Push plug and cable through under the sample compartment cover Lay the cables in the groove in the SPECORD Take care that the sample compartment cover does not squeeze the cables
13. e Peltier temperature controlled 6 cell changer with heat exchanger e Peltier temperature controlled 8 cell changer with heat exchanger Temperature control is through a separate temperature control unit fitted to the corresponding cell holder or cell changer respectively However the connection and the operation of each of these units is the same For a description refer to Section 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 53 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 13 1 54 Peltier temperature controlled cell holder air cooled ee EEE _ FO 1 Peltier temperature controlled cell holder 2 Electric cables between control unit and cell holder 3 Temperature control unit Fig 13 1 Peltier temperature controlled 1x cell holder with control unit The Peltier temperature controlled cell holder permits the temperature of cells of 12 5 mm x 12 5 mm x 45 mm 46 mm size L x W x H and 10 mm pathlength to be controlled Temperature control of the cell holder is performed via a separate control unit The rear side of the Peltier elements is air cooled through a heat transfe
14. try to release it by slightly turning it When it becomes already visible at the other end of the duct bend it to the opening e g by means of a pen 2 Place the cassette sipper system onto the carrying rails in the sample beam of the sample compartment so that the cell holder faces the detector In this position clamping lever Fig 1 1 11 points to the back 3 To position the flow cell as close to the detector as possible push the sipper system to the right against the sample compartment wall 4 Clamp the sample holder by means of the clamping lever User s Manual SPECORD 200 205 210 250 Accessories 07 2005 99 Analytik Jena AG Cassette sipper Thread the sample aspirating tube through one of the openings in the front wall Fig 1 1 12 Take care not to fold the tube The tube has a particularly smooth surface to avoid gas nucleation centers At tube folds however gas bubbles may form When these bubbles get into the sample cell they will strongly distort the results Lead the interface cable for connection to the SPECORD underneath the rear carrying rails to the connectors in the sample compartment wall and plug its plug into one of these connectors 14 3 3 Adjusting the flow cell 100 For the first use of the cassette sipper and after a change of the flow cell it is advisable to adjust the cell in the beam 1 First check the passage of non dispersed white light through the cell To this end se
15. 13 17 Front panel of temperature control unit Indicators for heat exchanger does not apply to air cooled Peltier temperature controlled cell holders The indicator LED Fig 13 17 9 located on the front panel of the control unit indicates the three possible states of the heat exchanger LED off No heat exchanger available or the heat exchanger has not been connected to the control unit via the 6 pin connector LED red 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 91 Analytik Jena AG Peltier temperature controlled cell holders cell changers Connection and operation of temperature control unit Pre selecting the temperature on the temperature control unit Caution In selecting the nominal temperature consider that this value always refers to the block temperature Depending on the temperature in the sample compartment the type of cell used as well as the type and volume of the sample material different end values of the temperature inside the cell may result and also different times for reaching these values Fig 13 18 1 Press the PGM button Fig 13 17 6 On the cell holder or cell temperature display Fig 13 17 3 it appears SP 1 2 Press the decrement button Fig 13
16. 17 4 to reduce the pre selected temperature or the increment button Fig 13 17 5 to increase it 3 Confirm the pre selected temperature by pressing the PGM button Fig 13 17 6 After two seconds the selected value will automatically be stored ae Note The nominal temperature can only be varied within the permissible temperature range 4 Exit the programming mode by pressing the EXIT button Fig 13 17 7 iC 38 M y 37 36 35 34 33 3ml H20 Quartz 1x1 block temperature 3ml H20 Quartz 1x1 cell temperature 32 3ml H20 Plastic 1x1 block temperature 3ml H20 Plastic 1x1 cell temperature 31 2ml H20 Plastic 1x0 4 block temperature 2ml H20 Plastic 1x0 4 cell temperature 30 HH 7 l 29 28 am H 0 100 200 300 400 500 600 700 800 900 1000 S 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 92 User s
17. 3 of the sample volume has flown through the cell and 1 3 of the sample is in the aspirating tube before the cell That way the cell can be rinsed with the sample before the measurement and carry over errors be minimized 7 Enter the found optimum pump time in the measurement parameters of the XYZ sampler Users Manual SPECORD 200 205 210 250 Accessories 07 2005 111 Analytik Jena AG Fiber coupling for measuring probes 16 Fiber coupling for measuring probes 16 1 Description and use The fiber coupling provides optical connection of measuring probes with their optical fibers to the SPECORD It allows samples to be analyzed outside the sample compartment The operating range of the optical fibers is from 220 nm to 1100 nm A Caution Aging of optical fibers by exposure to UV radiation Please note that optical fibers may be damaged in the long term if used at wavelengths below 220 nm That is why you should use them only in the wavelength range above 220 nm 16 2 Design and function of fiber coupling with measuring probe 3 1 Adapter for coupling light in out 6 Holder 2 Optical fiber for coupling light in 7 Setscrew for vertical adjustment 3 Optical fiber for coupling light out 8 Knurled screw 4 Measuring probe schematic 9 Slit position 5 Spring loaded handle 10 Adapter 1 schematic Fig 16 1 Fiber coupling adapter with measuring probe The fiber coupling consists of adapter 1 which couples out the light fro
18. EAE Ea raea Eaa TEE E 30 6 cell changer thermostatted cesscsseeeeeseeeeeeeees 31 DESCrIDUONaNnG USE a a a ee eee N 31 DESIO oae a O E A A 32 Installation and insertion in sample ComMpartMeNt cccccsseeeeeseeeeeseeeeens 33 Installation Of magnetic STIFPEVS cccccccceeececeeeeecceeseecceueeeceaeeessegeeeesaneeeseaes 33 Connection to a thermostat csesssseeeeeeeeeeeeeeeeeeeaaeesseeeeeeeeeeeeeeeeeeeeeeeaaaas 34 Installation in Sample compartment ccseeccecseeeeeceeeeeeeeeeeeeseeeeesseeeeeseeeeeens 35 OCI ANON re tec hela ieuecert eS ese te hee a aE 36 Settings in Measurement Parameters WINCOW c ccccceceseeeeeeeeeeeeeeeeeseeeees 36 Measurements with the 6 Cell CHANGED sccccccseeeeeeeeeeeeeeeeeeseeeeeseeeeessees 38 Operating modes of Cell CNANGENS ccccsssecccccsesecececeeeeceeeseeeeeesseeeeeeessaeess 38 S COICNAN GCMs lt nar ccctecca scour cesescca cesarean vacssccusidsvsdesdeest 41 Removal of transport lock on non temperature controlled 8 cell changer 41 DESIGN Ol S COll CNANOS lasera tool lv ergs macrulareeclenantiiwiate tee EANAN 42 Installation of 8 cell changer i issivseicot oeedieciacteeeer es PAs artes aed 42 Operation of the 8 Cell changer c ccccceeeeeccceeeeseeeeeeeeceeeseeeeeeeeeeeessaaaeeeeeess 44 SOlMWALS Seling Saaie a e N 44 Measurements with the 8 cell CHANGED cscsccccseseeeceeeeeceeeeeeceeeeeeseneeesaees 45 Us
19. Lay all connection cables and tubes for connection to SPECORD fluid thermostat and or magnetic stirrer so that they do not project into the beam in the sample compartment 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 8 cell changer 1 Connection cable for control unit of stirrer 2 Recess in sample compartment wall with plastic foam stopper 3 Connection to SPECORD 4 Water tubes 5 8 cell changer 3 4 _ Fig 11 1 8 cell changer installed in sample compartment of SPECORD 1 Mount the carrying rails in their bottom position gt Section Changing the position of the carrying rails p 8 Replace the plastic foam stopper 2 in the rear recess of the sample compartment by the plastic foam strips supplied along with the accessory Thread the cable of the magnetic stirrer under the rear carrying rails and push it through between the two plastic foam strips in the recess in the sample compartment In doing so 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 Thread the cable through underneath the cover of the sample compartment Make sure the cable is not squeezed when the cover is closed Connect the cable to the magnetic stirrer Conect the contr
20. Put the cell onto any desired position Take the connector Fig 13 11 2 from the storage receptacle Fig 13 11 4 and plug the connector onto the cell measuring sensor On the temperature control unit switch the selector switch to cell 4 lf you no longer need the cell sensor disconnect it from the connector and plug it into the storage receptacle Fault indication If the temperature displays Fig 13 17 2 and 3 on the control unit are flashing either the cell measuring sensor has not been connected properly to the connector or the sensor is defective Operation without heat exchanger When operating the Peltier temperature controlled 6 cell changer without heat exchanger or with the heat exchanger switched off cooling is electronically suppressed heating however is possible In this case if the ambient temperature is constant and the selected nominal temperature is about 5 degrees above sample compartment temperature the selected nominal temperatures can be kept to an accuracy of 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer Operation with pu
21. This holder accommodates round cells or ampoules cell test or test tubes Cell diameter 12 mm to 20 mm Cell height 40 mm to 70 mm Minimum filling level 20 mm 6 2 Description Support Round cell Spring rocker Vee guide AOU N Fig 6 1 Holder for round cells 6 3 Using the holder for round cells 1 Plug the holder for round cells from top onto the mounting plate for cell holders User s Manual Instrument Description Fig 8 Item 4 in the front beam path 2 Carefully withdraw the spring rocker 3 3 Slide the round cell 2 down along the vee guide 4 between support and spring rocker 4 Carefully let spring rocker return to hold the cell Ta Note Some manufacturers of cell tests provide round cells with a line mark Position round cells of this type in such a way that the line mark is aligned to the sample beam axis 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 19 Analytik Jena AG Holder for semi microcells and microcells 7 Holder for semi microcells and microcells 7 1 Description and use Semi micro and microcells have the standard outside width of 12 5 mm but a reduced inside width or filling aperture of 1 to 4 mm This requires accurate alignment of the cell to the sample and if necessary to the reference beam of the SPE
22. back put the adapter through this opening Close the opening again with the lid 3 Insert the adapter in the adapter holder 4 Put the optical fibers between the plastic strips in the opening for the optical fibers Fig 1 1 5 in the sample compartment 5 Close the sample compartment cover taking care that the optical fibers rest in the groove of the device cover under the sample compartment cover The optical fibers must not be squeezed by the cover 16 5 Alignment of fiber coupling 114 If the fiber coupling is used for the first time the adapter with its holder will have to be aligned in the beam path 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 17 Absolute Reflectance Attachment 17 1 Description and use Absolute Reflectance Attachment With this accessory you can determine the absolute reflectance of reflecting layers The layers must be homogeneous smoothly polished and have a constant thickness This accessory accommodates samples of a size between 40 x 40 mm and 70 x 70 mm and a thickness of 1 20 mm The angle of reflection is 7 17 2 Design Sample Sample locating plate Carrier for swivel mirror S
23. cell sensor in storage receptacle Connectors for connection to temperature control unit Connector for connection to SPECORD S600 Connector for connection to heat exchanger Stepper motor drive with lead screw Knurled screw for clamping the unit to the carrying rails Water tubes for connection to the heat exchanger O ON OOF WD Fig 13 9 Design of Peltier temperature controlled 6 cell changer User s Manual SPECORD 200 205 210 250 Accessories 07 2005 73 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 13 3 5 Installation of the Peltier temperature controlled 6 cell changer 74 OoOonN DOF WD 1 6 Knurled screws for fastening the cover prop Hole with slot in sample compartment cover Electric cables from cell changer to temperature control unit and to heat exchanger Recess with plastic foam stopper in sample compartment wall 9 pin connector for connection to SPECORD Coolant tubes Knurled screw for fastening the cell changer to the carrying rails Peltier temperature controlled 6 cell changer Connector of temperature sensor in storage cavity Fig 13 10 Installation of Peltier temperature controlled 6 cell changer in the SPECORD Lay connection cables tension free The connecting cables and the coolant tubes must be laid without tension and in a way that they do not hinder the movement of the cell changer while in operation Make s
24. control unit 2 Heat exchanger 3 Peltier temperature controlled 8 cell changer Fig 13 1 Peltier temperature controlled 8 cell changer The cell changer is an automatic sample changing system Its driving unit with stepper motor drive is controlled by software Temperature control of the cell holder is performed via a separate temperature control unit The coolant circuit of the heat exchanger keeps the rear side of the Peltier elements at a temperature near the ambient temperature The controlling sensor used is a Pt100 measuring sensor located in the upper part of the cell block In addition to the controlling sensor the cell holder contains two further Pt100 sensors for optional monitoring of either the holder or the cell temperature The cell holder contains eight positions for cells having a pathlength of 10 mm and external dimensions of 12 5 x 12 5 x 45 L x W x H in mm The cell sensor is specially designed for standard cells with round PTFE stopper It may remain in the cell during the analytical measurement Cm Note When using other cells the immersed measuring sensor may project into the sample beam thus distorting the measurement results Optionally the 8 cell changer may be factory equipped with a magnetic stirrer The Stirring speed is adjusted at the temperature control unit You can also use two Peltier temperature controlled 8 cell changers in combination to increase the number of samples that can be measured to a maxi
25. cotton swab soaked with distilled water and curd soap Don t exert any pressure in wiping Then wipe with a new cotton swab soaked with distilled water only Finally dab metal mounts dry e Carry and store the absolute reflectance attachment only in a closed box 18 9 Technical data Angle of reflection Graduation of angular scale Accuracy of angular adjustment Vignetting of beam in angular range 11 15 Maximum sample thickness Illuminated sample area on adjusted angle of reflection User s Manual SPECORD 200 205 210 250 Accessories 07 2005 123 Analytik Jena AG Integrating Sphere 19 Integrating Sphere 19 1 Description and use The integrating sphere is suitable for the measurement of transmittance and diffuse reflectance of scattering solid or liquid samples on these spectrophotometers In diffuse reflectance measurements the measuring geometry of the sphere is 8 d Consider that due to the effect of the sphere the level of the measured signal drops to a small percentage compared to the optical path without sphere This means that you can take measurements at a high accuracy only with an absorbance of up to about 2 A The integrating sphere with a sphere diameter of 75 mm consists of two Spectralon hemispheres with apertures for beam entrance and exit beam reflecting optics and holders for samples and cells for transmittance and diffuse reflectance measurements It is inserted in the optical path of
26. desired measurement parameter record in WinASPECT software For the reflectance measurements choose the following accessory specific options Measurement Option to be activated parameter Correction Reference Display Reflectance Accessory Reflectance fixed angle 2 Take the reference measurement For that set the reflectance attachment to the V beam configuration shown above 3 When the reference measurement is finished turn the unit to set it for W beam configuration 4 Withdraw sample holder 10 from sample locating plate 2 insert the sample 1 and let the sample holder return to the sample 5 Take the sample measurement User s Manual SPECORD 200 205 210 250 Accessories 07 2005 117 Analytik Jena AG Absolute Reflectance Attachment Calculation of reflectance The measured reflectance R is calculated from the sample measurement reference measurement ratio Tsample Rsample Sample measured in W configuration R r Reference Reference measurement in V Reference configuration i Irs Intensity after reflection at the letren reference mirror reference beam o E Tse x PR x i Ipsi Intensity after the first reflection at the Isample sample Reference beam Ipsi2 Intensity after the second reflection at the sample The result of the measurement is R Ipsi X Ipse If the sample is sufficiently homogeneous it applies Ips Ips2 The absolute reflectance of t
27. ect a a aea 62 13 2 2 Technical data of Peltier temperature controlled cell holder with heat Exchande erea ance ade catnatyndaten tec dated tae Green tact tavgacieco tase e 64 13 2 3 Design of Peltier temperature controlled cell holder with heat exchanger 66 13 2 4 Installation of the cell holder in the SPECORD c cccceceeeseseeeteeseeeees 66 13 3 Peltier temperature controlled 6 cell CNANGEL c ccccceececeeeeeeeeesseeeeseeees 69 13 3 1 WIS a E EE EE EEEE EEE PEE E T AEE E EEE T ETE E E 69 13 3 2 oer 910 eean a rE ere OE 70 13 3 3 Technical data of Peltier temperature controlled 6 cell changer 71 13 3 4 Design of Peltier temperature controlled 6 cell CNANGEL ccccseeeeeeseeeeees 73 13 3 5 Installation of the Peltier temperature controlled 6 cell changer 0 74 13 3 6 Settings in WINASPECT Software ccccscscseseseseseseresesesseveveceseresereneneeteveveven 77 13 9 7 Measurement procedure os 2ccctccdncdelac Srelstindecgwiareaseptantesduliveadededendesxehureesantlecvens 78 13 4 Peltier temperature controlled 8 cell CHANQEL cccccseeeeeeeeeeeeeeeeeesseeeeeens 79 13 4 1 SENAN OS athe EE EA E EE A 80 13 4 2 Technical data of Peltier temperature controlled 8 cell changer 0 81 13 4 3 Design of Peltier temperature controlled 8 cell CNANGEL ccccseeeeeeeeeeeees 83 13 4 4 Installation of Peltier temperature controlled 8 cell changet
28. integrating sphere is shown in that position it is inserted into the SPECORD for reflectance measurements of powdery samples vertical arrangement With this arrangement the reflectance sample is located underneath the sphere body The sphere body may also be inserted swiveled by 90 horizontal arrangement for transmittance measurement of solid or liquid samples in cells It is placed with its locating surfaces 14 15 or 16 onto the carrying rails in the sample compartment of the SPECORD 126 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Integrating Sphere 19 3 Measurements with the integrating sphere In transmittance or diffuse reflectance measurements the sample is brought into direct contact with the sphere In this way the sample presents a part of the inner sphere surface thus affecting the efficiency of the sphere So for instance in transmittance measurement the radiation is weakened by the absorption in the sample As the sample itself however is part of the sphere the sphere efficiency changes depending on the reflective or reflectance properties of the sample This means that the efficiency of the sohere depends on sample properties This dependence results in a non linear functional relation between sample absorbance and the measured signal For high precision measurements it is therefore advisable to take this non linear relation into account by calibrating the system b
29. isopropanol 13 6 2 Connecting the heat exchanger 1 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 94 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Connection and operation of the heat exchanger 2 Connect the power cable to the power input connector Fig 13 20 3 and then toa power outlet 3 Slip the tubes from the cell holder changer over the appropriate tube connectors of the heat exchanger Fig 13 19 3 and lock them in place by turning the knurled nuts anti clockwise 4 Remove screw cap Fig 13 19 1 by turning it anti clockwise 5 Switch on the heat exchanger with power switch Fig 13 20 1 6 Fill the prepared coolant through the opening in the compensating tank Fig 13 19 2 until the filling level is approximately 1 5 cm below the top edge of the compensating tank and the coolant circuit is free of air bubbles no bubbles rising in the tank and a noise free circulation of the coolant 7 Close the compensating tank hand tight with the screw cap Note When installing the heat exchanger please consider that the maximum delivery head of the device is approximately 1 2 m Depending on the place of installation of the heat exchanger the laying of the tubes and for technical reasons it may happen that air c
30. left 7 Thread the interface cable through underneath the rear carrying rails and connect ists plug to the left connector in the back wall of the sample compartment Adjustment of the cell changer The cell changer can be adjusted computer controlled to optimally position the cells in the beam Adjustment is necessary e At the first use of the cell changer e After wavelength calibration e After relocation of the SPECORD e When working with microcells 1 Install the empty cell changer in the sample compartment 2 Onthe Accessories tab activate the 6cell changer option 3 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 If you intend to use microcells in the analyses insert a microcell filled with water in every of the six positions 4 Start automatic adjustment by a click on the Adjustment button 10 4 Operation 10 4 1 Settings in Measurement Parameters window 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 36 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 6 cell changer thermostatted Cell changer First sample m No 1 Pos 1 Last sample moj ERE Fos 1 1st sample Reference Manual Start T Adjustment Slow time scan _ P
31. magnetic stirrer Magnetic stirrer and thermostat connectors must be factory fitted and cannot be retrofitted In addition a Peltier temperature controlled 8 cell changer is available Section Peltier temperature controlled 8 cell changer p 79 11 1 Removal of transport lock on non temperature controlled 8 cell changer The non temperature controlled cell changer is protected in transport by a red plastic foam pad under the cell block Transportsicherung Transport lock Fig 11 1 Transport lock on non temperature controlled 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 41 Analytik Jena AG 8 cell changer 11 2 Design of 8 cell changer 7 6 5 1 Cell block with insulation 2 Stepper motor drive 3 Connecting cable for connection to stirrer control unit 4 Stirrer control unit 5 Connecting cable for connection to SPECORD 6 Water tubes for connection to thermostat Fig 11 2 8 cell changer 11 3 Installation of 8 cell changer 42 This section describes the installation of the 8 cell changer with connection to a fluid thermostat and a magnetic stirrer If your cell changer does not have these additional components you can skip this part of the description Caution Lay cables and tubes properly
32. numbered consecutively e Every illustration has its own caption e Steps of operation are consecutively numbered e Cross references are marked by an arrow e g gt Section Introduction p 1 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 5 Introduction Safety notes 1 1 Safety notes A gt D Handling of the accessories is subject to the safety instructions given for the SPECORD basic unit gt User s Manual SPECORD Section Safety Notes For all accessories of the SPECORD Series the following safety instructions are applicable Intended use The SPECORD including original accessories may only be used for the applications described in this manual The manufacturer cannot assume any liability for any other application including that of individual modules or single parts This also applies to all service or repair work that is not carried out by authorized service personnel All warranty claims shall be forfeited Transportation and storage Accessories not in use should always be stored in the provided packaging For transportation always use the provided original packaging Risk of corrosion Do not set up the device near aggressive vapors e g strongly corrosive acid or caustic vapors The vapors might corrode the connections mechanical and optical components of the device Avoid exposing the sample compartment and the accessories to strongly corrosive substances For the ana
33. of the cells to the sample beam Optional cell changer equipment The 6 cell changer can be equipped optionally with magnetic stirrers 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 31 Analytik Jena AG 6 cell changer thermostatted 10 2 Design fo 6 1 Interface cable 5 Cell holder with thermostatting jacket 2 Clamping lever 6 Connector for magnetic stirrer 3 Support for cell holder 7 Driving unit with stepping motor 4 Quick lock couplings for coolant inlet Fig 10 1 Thermostatted cell holder and driving unit 1 4 1 Holder for magnetic coils of stirrer 3 Magnetic coil under measuring position 2 Flat cable 4 Magnetic coil under the next position Fig 10 2 Thermostatted cell holder with magnetic stirrer 32 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 6 cell changer thermostatted 10 3 Installation and insertion in sample compartment 10 3 1 Installation of magnetic stirrers 4 1 1 Stirring magnet 5 Adapter 2 Carrier for stirrer coils 6 Connector on power supply 3 Flat cable 7 Power supply 4 Connectors of flat cable 8 Speed control Fig 10 3 Installation of magnetic stirrer Caution Incorrect line voltage may damage the unit Make sure the op
34. order adjustment white undispersed light passes through the sample compartment This high intensity beam is particularly suitable for the alignment of accessories Open the Service Check utility of WinASPECT software by following this procedure 1 On the Windows taskbar click the Start button In the Programs folder open the WinASPECT folder There click on Service xxx This will bring up the Specord xxx Service Check dialog box 2 In this dialog box click on the Zeroth Order button and choose the halogen lamp HL Lamp 1 3 3 Changing the position of the carrying rails 1 2 3 4 1 Knurled screw 3 Adapter 2 Support in sample compartment wall 4 Carrying rail Fig 1 2 Carrying rails mounted in bottom position To use the cell carousel you have to mount the carrying rails in the bottom position For that you need two adapters which are included in the equipment of the cell carousel 1 Unscrew one of the carrying rails in the sample beam path front pair and remove the rod from the sample compartment 2 Screw one adapter 3 onto the carrying rail 3 Put the carrying rail onto the bottom cone shaped journal in the right hand sample compartment wall 8 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Introduction Basics of SPECORD alignment Hold the carrying rail with adapter from the bottom against the support 2 and fasten the carrying rail by means of the knurled screw F
35. room air when running analyses at low temperatures 13 4 5 Settings in WinASPECT software 88 The cell changer is controlled by WinASPECT software On the Accessories tab of the measurement parameter window choose the 8 cell changer option Cell changer First sample Ho 1 Pos 1 Last sample Ho 3 Pos 1 1st sample Reference z Adjustment Manual Start T Slow time scan D Parking Fig 13 15 Options for Peltier temperature controlled 8 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 1 sample reference The sample placed on the 1 position selected above is treated as reference In this case it is not necessary to run the reference measurement separately The reference measurement will be performed within the normal sample measurements Start manually 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer measurements The measurement in the respective cell will be started only after you added the starting substance Slow time
36. smoothly Successively turn the screws for vertical adjustment 4 and the screws for horizontal adjustment 6 Check the adjustment by taking an energy measurement In these measurements take care to always keep the sample compartment cover closed 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 6 cell changer thermostatted 10 6 cell changer thermostatted 10 1 Description and use The six cell changer is an automatic sample changing system that is connected to and controlled through the SPECORD Temperature control is by means of a water thermostat It consists of two separable modules e athermostatted cell holder e adriving unit with stepping motor drive The cell holder has six positions for the accommodation of 10 mm pathlength cells of the following outer dimensions 12 5 x 12 5 x 45 Lx Wx Hin mm The cell holder is equipped with a quick lock tube coupling allowing drip free connection and disconnection of the thermostatting tubes The stepping motor drive of the driving unit moves the cell holder within approx 1 s to the next position In combination with an optocoupler defining the initial and the end points of the motion range it ensures exact and reproducible alignment
37. the SPECORD sample compartment For loading powdery samples it may be removed from the sample compartment and reproducibly reinserted Caution Observe the following conditions of use With its uncovered mirrors and high reflectivity Spectralon components the integrating sphere is a very sensitive optical device Especially when handling powdery samples take care to avoid that powder or other dirt particles get into the sphere and thus reduce their reflectivity A decrease in reflectivity of the Spectralon units from 99 to 98 will result in a reduction to half of the standard efficiency of the integrating sphere The Spectralon inserts and the gloss trap too should be treated with the same care as the efficiency of the unit will also be reduced by a decrease in the reflectivity of these components Unpacking Carefully remove the sphere body from the transport and storage box taking care not to touch the mirrors Hold the sphere body only at the side plates Storage In periods of non use of the integrating sphere store it along with all its accessory items in the corresponding box Though the mirrors carry a protective coating of SiO2 you should protect them from contamination Besides take care that you remove the reflector from the SPECORD if you do not use the integrating sphere Otherwise its bright aluminum surface might be affected Cleaning Despite all care it may become necessary to clean the mirrors particu
38. with the cell changer in the reference beam Both devices may be operated from the same thermostat or cryostat For this mode a corresponding set of tubes is available You can insert flow cells in the thermostatted cell holder used in combination with the sipper system 8 2 Description Inlet connector Outlet connector Thermostatting tube inlet Thermostatting tube outlet Os o NOOO FR WD Sleeve nut Guide Knurled screws for magnetic stirrer 8 Cell 9 Aperture Fig 8 1 Thermostatted cell holder 8 3 Using the thermostatted cell holder 8 3 1 Connection and installation in sample compartment 1 Thread the coolant tubes from the interior of the sample compartment through the tubes in the right hand sample compartment wall of the SPECORD Fig 1 1 6 The tube ducts in the wall are provided with steps to achieve a higher light tightness 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 25 Analytik Jena AG Thermostatted cell holder 8 3 2 26 Connect the thermostatting tubes 3 4 between the tube connectors 1 2 of the thermostatted cell holder and the corresponding connectors on the external fluid thermostat The tubes have an inside diameter of 4 mm and a wall thickness of 1mm The tubes are transparent
39. without touching it 6 Put the sample rack onto the base covering The rack rests on the conical plug and the stop strips on the base covering 7 Insert the rinse vessel if required Further installation procedure for the APG 100 model Use the upgrade kit for the installation of the APG 100 3 Push the four longer feet into the foot sockets and fasten the feet with the knurled screws 4 Put the XYZ autosampler upright on the table and check its stability Readjust the feet if necessary 4 In place of the stirrer bracket of the APG 53 slide the adapter with the duct for the sample tube onto the underside of the Z dome into the grooves Tighten the knurled screw 10 5 Put the base covering from the front onto the basic device and fasten it by means of the four bolts 2 6 Put the sample rack onto the base covering The rack rests on the conical plug and the stop strips on the base covering 15 4 Connecting the XYZ autosampler to the SPECORD 108 1 Set up the autosampler to the right of the SPECORD keeping a minimum spacing of 10 cm 2 Use the provided cable to interconnect the 15 pin connector 16 of the XYZ autosampler and the connector labeled APG on the right side of the SPECORD 3 Verify that the operating voltage setting of the XYZ autosampler label on 19 agrees with the available line voltage 4 Connect a power cable to mains input connector 20 Then connect this cable to a power outle
40. 0 Line fuses for WC 601 EMC jamming and noise immunity as per DIN EN 61326 and 61326 A1 Fire resistance of the case of the heat exchanger according to UL94 Protection Type Coolant Maximum delivery head Operating temperature range Transport and storage temperature range Relative humidity Overview 13 11 Technical data of heat exchanger 3 2 kg 225 x 175 x 200 mm 220 240 V 15 10 50 Hz 50 VA 2 x T 0 5 A H 250V Type 19181 Wickmann 2 x T 1 6 A H 250V Type 19181 Wickmann The device can be installed and operated in all environments HB 1 6 IP 20 Approximately 0 4 distilled water with an addition of 4 ml isopropanol 1 2m 15 4 35 C 40 C 60 C Up to 90 at 30 C 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 13 4 3 Design of Peltier temperature controlled 8 cell changer 1 3 4 5 Cell block with insulation Stepper motor drive Connector for cell sensor in storage receptacle Connectors for connection to temperature control unit Connector for connection to heat exchanger Connector for connection to SPECORD Water tubes for connect
41. 2 Universal Dolder aaa a eas te rc teces ocncecse eecsateccereesesencuseeces 11 2 1 Description and US Ci cte pied asec E sna nceniae irae teacaeee ancasteeeeeee 11 2 2 PS SCHIOUON alane seeseasaceecientee E ee teecuseaecoateen sateen en eee 11 2 3 Using the universal NOlder cccccccccssseececceeeseceeceeaeeceeeeeaeeeeessuageeesseaageeess 12 3 100 mm cylindrical cell absorption tube 13 3 1 Description and USE oerien a incre a Eea E RA E ERARE 13 3 2 DGS CIOUON xiaset actin cencectatan a a Sentencenae lead Cenaeeens 13 3 3 Inserting the 100mm cylindrical Cell cccccccseeeeeceeeeeeseeeeesseeeeeseeeesseeeeeeas 13 3 4 Care and transportation of cylindrical Cell ccccccceseeececeeeeeeeseeeeeeeeessaeeeees 14 4 Sold sample holder ieee ees 15 4 1 p scnipion and USE ssr E aAA AA ENa 15 4 2 Using the holder and inserting the sample ccccseeeceeeeeeeeeeeeseeeeeeeesaeeeeees 15 5 Holder for cylindrical CellS ccssscsseseeeeeeeeeseeeeeenees 17 5 1 DESCrIDTOM ANG USC srg elect ste a eaten unet ae eo E 17 5 2 BB Yeo er 01 8 meee eeee me int omer remeron rev OES rn oe ME Te eee oe 17 5 3 Using the holder for cylindrical cells cccccseeececeeeeeeeeeeceeeeeeeesseeeeeeesaaeeeees 17 6 Holder for round cells Tiinaa 19 6 1 Description and US Coie cere tee ser sce ettes cnc crevs rns casteesctsvaseecieedaeatraus meen payee taresneeets 19 6 2 Byeicvel d 6 3 9 ieeenteemee
42. 7 Plug the plug of the flat cable 5 into the connector 6 of the power supply with speed control 7 8 Connect the power supply to a power outlet 9 Insert the thermostatted cell holder with magnetic stirrer exactly in the same way as the thermostatted cell holder without stirrer 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 27 Analytik Jena AG Adjustable cell holder thermostatted 9 Adjustable cell holder thermostatted The adjustable thermostatted cell holder accommodates a cell of 10 mm pathlength and the following external dimensions 12 5 x 12 5 x 35 L x W x Hin mm The height of beam transmission is 15 mm The holder is designed for the accommodation of cells with very small window apertures e g 1mm on HPLC cells It provides defined location and hold in and alignment to the beam With such small apertures even minimum misalignment of the cell may impair the signal to noise ratio orWwWNDN Fig 9 1 Adjustable thermostatted cell holder i A A Ai Fig 9 2 HPLC cell User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Sample feed Sample aspiration Beam aperture Screws Lid Tube connector with sleeve nut Screws for vertical adjustment Screws to fasten the cell holder 4th scr
43. 8 The contact cap is fixed in the cover cap with a grub screw By loosening this screw you can vary the immersion depth of the contact pins in the cover cap by maximally 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 13 3 Peltier temperature controlled 6 cell changer 13 3 1 Use The cell changer is an automatic sample changing system Its stepper motor driving unit is driven by the software Temperature control of the cell holder is performed via a separate temperature control unit The coolant circuit of the heat exchanger keeps the rear side of the Peltier elements at a temperature near the ambient temperature The controlling sensor used is a Pt100 measuring sensor located in the upper part of the cell block In addition to the controlling sensor the cell holder contains two further Pt100 sensors for optional monitoring of either the holder or the cell temperature The cell holder contains six positions for cells having a pathlength of 10 mm and external dimensions of 12 5 x 12 5 x 45 Lx Wx Hin mm The cell sensor is specially designed for standard cells with round PTFE stopper It may remain in the cell during the analytical measurement a Note When using other cells the immersed measuring sens
44. CORD Three cell holders are available that meet this requirement for precise alignment to the beam 1 The non adjustable holder with a fixed mask of 2 5 mm diameter for semi microcells of glass or quartz and a beam height of 8 5 mm 2 The non thermostatted holder for glass or quartz microcells with black sidewalls This holder is adjustable both vertically and at right angles to the beam axis The beam heights possible are 8 5 mm and 15 mm 3 The non thermostatted holder for glass or quartz microcells with black sidewalls This holder is adjustable at right angles to the beam axis The beam height is 8 5 mm 7 2 Holder for semi microcells Pathlength of semi microcell max 10 mm Height of beam center 8 5 mm External width of cell 12 5 mm Minimum filling level 15 mm Fig 7 1 Holder for semi microcells 1 Slip this holder onto the mount for cells Fig 1 1 10 or the universal holder gt Section Universal holder p 11 and push it down as far as it will go 2 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 21 Analytik Jena AG Holder for semi microcells and microcells 7 3 Adjustable holder for microcells non thermostatted 8 5 mm 15 mm beam height am 4 5 1 Handle 2 Spring 6 3 Holder 2 4 Screw for vertical adjustment 5 Thrust pad 6 Knurled screw 7 Slit positi
45. Fig 13 4 Sample compartment cover with cables threaded through 0008 59 Fig 13 5 Bottom of Peltier temperature controlled 1x cell holder cceee 61 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 135 Analytik Jena AG Figures 136 Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig 13 6 13 7 13 8 13 9 13 10 13 11 13 12 13 13 13 14 13 15 13 16 13 17 Fig 13 18 Fig 13 19 Fig 13 20 Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig Fig 14 4 14 2 14 3 14 4 15 1 15 2 15 3 16 1 17 1 17 2 18 1 18 2 18 3 18 4 19 1 19 2 19 3 19 4 Peltier temperature controlled cell holder with heat exchanger 66 Cell temperature measuring Sensor PT 100 cccecccceeceeceeeeeeeeeeeeeaees 68 Peltier temperature controlled 6 cell changer with SPECORD 210 69 Design of Peltier temperature controlled 6 cell Changer cccceee 73 Installation of Peltier temperature controlled 6 cell changer in the SPEC O AD ace a A ee 74 Cell measuring sensor for the Peltier temperature controlled CONC hange cs ccaahe pet a a codes as accent ae een ee sede ceeeeeee 76 Options for Peltier temperature controlled 6 cell changer for SPECORD 77 Design of Peltier temperature controlled 8 cell Changer cccceee 83 Cell measuring sensor for the Pel
46. G 100 For cleaning the flow through system rinse liquid can be aspirated from a rinse vessel 15 2 Safety notes AN Warning Electric shock Prior to opening the device switch it off and disconnect the power plug Take care that no liquids get onto cable connectors or into the electrical system of the device Proper earth conductor Connect the power cable only to a properly installed power outlet with earthing contact to ensure protection as per Protective Class protective multiple earthing Do not use an extension cable without earth conductor as this would make the protection ineffective If you use multiple socket connectors make sure the permissible earth current is not exceeded Make sure the power cables are free from defects Correct line voltage Prior to connecting the XYZ autosampler to a power outlet make sure the operating voltage specified on the rating plate on the rear panel agrees with the local line voltage Operation on other than the specified line voltage may destroy the device The device may be converted for use on other line voltages only by service staff Risk of accidents Mind the motion range of the guiding arm of the uptake tube While the device is in operation there is the risk of accidents Do not put your fingers into the guiding aperture of the arm while the device is operating Observe the operating manual Additionally observe the instructions and advice given in the accompan
47. Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Connection and operation of temperature control unit 13 5 3 Replacing fuses on the temperature control unit Replace any blown fuses on the temperature control unit by following this procedure 1 Disconnect the power cable 2 Open the fuse holder by pulling its lid 3 Replace the defective fuses considering the technical data of the cell holder or the cell changer you are using 4 Close the fuse holder again 5 Reconnect the power cable 6 Switch the SPECORD on again User s Manual SPECORD 200 205 210 250 Accessories 07 2005 93 Analytik Jena AG Peltier temperature controlled cell holders cell changers Connection and operation of the heat exchanger 13 6 Connection and operation of the heat exchanger Heat accumulation Always keep ventilation slits free The warning 1 Danger Heat accumulation Keep free slits is located at the front panel of the heat exchanger 1 Screw cap 2 Compensating tank 3 Coolant tube connectors Fig 13 19 Heat exchanger front panel 1 Power switch 2 Fuse holder for line fuse 3 Power input connector 4 7 pole connector for temperature control unit 5 Type label Fig 13 20 Heat exchanger rear panel 13 6 1 Preparing the coolant In a separate vessel mix approximately 400 ml of distilled water with 4 to 5 ml of
48. T open the Device Driver 2 Choose the general measurement parameters slit wavelength ordinate display etc 3 Under Correction choose the Reference option or use a saved file Special option 4 On the Accessories tab choose either APG 53 or APG 100 depending on the sample rack used 53 or 100 samples ACCessary APG K3 Auto sampler Samples 2 Washing before measure Purnp time z Wash time s fi Reference na reference positions Fig 15 3 Accessories tab APG 53 selected Parameter Description Button Samples Number of samples placed on the sample rack including reference and wash solution Setting range for APG 53 1 53 Setting range for APG 100 1 100 Sampling always starts with rack position 1 Make sure to fill the tray consecutively without leaving any empty places in between Pump time s The pump time is the time needed for optimum transfer of the sample to the cell Setting range 0 300 s Wash before Executes a cleaning step between two sample measurements For every sample that the aspiration tube dips into the wash vessel When you enter a wash time this step includes the aspiration of the wash solution and rinsing of the sipper system Wash time Pump time for the wash solution Setting range 0 300 s Reference Use of one or several references on the sample rack After a click on Reference a small dialog box appears showing the list of samples Mark the tray position
49. a reflecting angle of 7 116 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Absolute Reflectance Attachment 17 5 Adjustment The Reflectance Attachment has been adjusted for the use on SPECORD 200 205 210 You can use it on these SPECORD models without any additional adjustment If you want to use a reflectance attachment already available it is advisable to check the adjustment of this unit For that follow this procedure 1 Place the reflectance attachment onto the two front carrying rails in the sample compartment Push it to the right hand wall of the sample compartment as far as it will go Clamp it in this position by means of clamping lever Fig 17 1 8 Set V beam configuration Adjust the zeroth order of the monochromator gt Section Adjustment of zeroth order p 8 Turn stop screw Fig 17 1 6 to adjust the unit so that the beam passes through the center of the cell receptacle for turbid samples thus being incident on the center of the detector surface Put a white screen e g a white paper strip in the cell receptacle for turbid samples To adjust the unit in W beam configuration put a flat mirror against the sample locating plate Fig 17 1 2 Then proceed as described above for the adjustment of the V beam configuration To adjust the unit turn stop screw Fig 17 1 5 17 6 Measurements with the Absolute Reflectance Attachment 1 Create the
50. analytikjena Accessories UV VIS Spectrophotometer SPECORD 200 205 210 250 A Analytik Jena AG analytikjena si i Konrad Zuse Str 1 07745 Jena Phone Hotline 49 3641 77 7407 Fax 49 3641 77 7449 e mail service analytik jena de General information about Analytik Jena AG on the internet htto www analytik jena de Copyrights and Trademarks Microsoft Windows 2000 Windows XP Windows NT MS Excel are registered trademarks of Microsoft Corp Publication No 221 426 23 Edition July 2005 Technical documentation made by Analytik Jena AG This documentation describes the state of this product at the time of publishing It need not necessarily agree with future versions of the product ETETETT Subject to change TUV CE CERT DIM EM Foi Oe oii boa 1 TCH Copyright 2005 Analytik Jena AG Contents Contents 1 NENEROGUICUIO Micrecesrcesecee ss teccerens ices ereaeui cer tvecerseessacensesen este tare 5 1 1 SAICLY NOLES A E E A A E EE EA T E A E EE 6 1 2 Gare OracCeSS ONES niid n ce denneacedeaeaees 7 1 3 Basics of SPECORD aliQnment ccccccseeeeccceeeeeeeeeeeeeeeeseaeeeeeeeeeseeaaeeeees 7 1 3 1 Sample compartment of SPECORD c cccccscscsesesesecesecesesereeceveveveveveveveceres 7 1 3 2 Adjustment OF zeroth order sess sed oro 2 ences catia apie da i ER ES RA 8 1 3 3 Changing the position of the Carrying rails ccccceccccecsseeeeeeeeeeeeeeeeseeeeeeeeeaeees 8
51. and warning labels Observe the type label and the warning labels on the devices Accumulation of heat Make sure that you do not cover the ventilation slots in the bottom plate and on the rear panel of the device as well as on the front panel of the heat exchanger Heat accumulation might result in overheating and faults on the equipment Ingress of water Take care to ensure that no liquids can get into the control unit to avoid any damage to the device Do not place the heat exchanger or containers with liquids onto the control unit 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 e DIN EN 61010 1 IEC 1010 1 e 73 23 EEC e 89 336 EEC User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 13 4 2 Technical data of Peltier temperature controlled 8 cell changer Operating principle Thermoelectric heating and cooling Cooling of rear panel of TEC Water cooled Guaranteed regulated temperature range at 25 C ambient temperature PTC 800 with heat exchanger WC 600 10 C 60 C PTC 801 with heat exchanger WC 601 5C 105 C Block temperature setting range PTC 800 with heat exchanger WC 600
52. ar as it will go If the clamping lever points upward it will hinder the motion of the sample tray Put the sample tray Fig 12 1 3 onto the corresponding support Fig 12 1 2 of the driving unit In doing so slightly turn the tray so that it engages in the guiding slot Fix the sample tray to the driving unit by means of the knurled screw Fig 12 1 6 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 Cell carousel 12 4 Operation The cell carousel is controlled via WinASPECT software In the Device Driver dialog box on the 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 51 Analytik Jena AG Peltier temperature controlled cell holders cell changers Operation 13 Peltier temperature controlled cell holders cell changers The following cell holders and cell changers with Peltier temperature control are available e Peltier temperature controlled cell holder air cooled e Peltier temperature controlled cell holder with heat exchanger
53. arking Fig 10 6 Accessories tab Cell changer For the control of the cell changer via WinASPECT the following options are available Parameter Description Button First sample Position of the first sample on the cell changer Last sample Position of the last sample on the cell changer 1st sample To be activated if the first place on the cell changer holds the reference reference In this case it is not necessary to take a separate reference measurement The reference measurement is then integrated in the normal sample measurement process Manual start If activated a small dialog box appears Start cycle OK The actual sample measurement is started only after you confirmed the request You can use this option for kinetic measurements The measurement in the respective cell will then be started only after you added a starting substance Slow time scan Activate this option if in cyclic measurement mode you want to measure all samples on the cell changer successively first Deactivate the Slow time scan option if in cyclic measurements you want to measure all cycles of one sample first before the cell changer moves to the next cell position Interval Accessible only if the slow time scan option has been activated The interval time is the time from the beginning of a cycle to the beginning of the next cycle Hence it also includes the time required for sample measurement Enter the desired interval time in th
54. art the sample measurement with the corresponding Start Measurement toolbar butto or menu command Measurement Measurement 10 4 3 Operating modes of cell changers 38 Beside the normal operating mode you can operate the cell changers in Slow time scan mode 1 2 6 1 2 6 E i E F a oe Cy ty J NS ag es ener eee Normal mode Slow time scan mode Fig 10 7 Cell changer Operating modes In normal mode first all cycles of a measurement are executed for the sample on a defined cell position before the measurement cycles of the sample on the next position are started For kinetic measurements this means that the complete reaction kinetic measurement is taken on one sample first before the next kinetic reaction is started requires Manual start check box to be activated In Slow time scan mode the reaction kinetic measurement can be optimized by measuring the samples cyclically in a time shared mode This means that in this mode the samples are measured successively in every cycle beginning with the sample on position 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 Tab Mode Accessories 6 cell changer thermostatted Settings Measuring mode Time Scan In this mode it is not possible to subdivide the total measuring time in several perio
55. asten the knurled screw hand tight so that the carrying rail cannot be moved Repeat the above procedure for the second carrying rail Users Manual SPECORD 200 205 210 250 Accessories 07 2005 9 Analytik Jena AG Universal holder 2 Universal holder 2 1 Description and use The universal holder accommodates the following accessory units e Holder for 100 mm cylindrical cell e Holder for cells of up to 50 mm pathlength e Thermostatted cell holder for accommodation and temperature control of a cell of up to 10 mm pathlength may be fitted with magnetic stirrer e Thermostatted cell holder for accommodation and temperature control of a cell of up to 50 mm pathlength e Solid sample holder for accommodation of films and sample plates of up to 25 mm pathlength and a minimum diameter of gt 20 mm e Holder for round cells e Holder for semi microcells and microcells 2 2 Description 1 Mounting plate for cell or solid sample holders 2 Clamp lever Fig 2 1 Universal holder User s Manual SPECORD 200 205 210 250 Accessories 07 2005 11 Analytik Jena AG Universal holder 2 3 Using the universal holder Fig 2 2 Attaching and clamping the universal holder 1 Put the universal holder with its hook onto the rear of the carrying rails allocated to sample or reference channel Then slide it to the right hand wall of the sample compartment as far as it will go 2 Throw clamp lever 2 to the right to clamp the uni
56. ceeesecseaseecseneeeesaeeeeseaeess 114 Absolute Reflectance Attachment ccsssseeee0 115 Description and It o ateeer serene rein See eieernree eee ein Rene te ener ee eee eee re 115 DESOT ictess casted enacted a a e A A 115 Installation in Sample compartment cceeecccseeeeecseeeeeeeeeeeeseeeeesaeeeessaeees 116 Operan Principesei R O OTE 116 AUSIN e a a ee 117 Measurements with the Absolute Reflectance Attachment 008 117 Care ANd maintenance ccccccccccccssseseeseeeeeeeeeeeeeeeeeeeauaescseeeeeeeeeeeeeeseeaaaaaas 118 Variable Angle Reflectance Attachment 119 Description and USE neheni kaa ia sete a Aaa ei a Eai 119 Design and operating principle ceccccccsseeceeeceeeeeeeeceeeeeeeseeeeeeeeesaeeeeeeesaaess 119 Installation in sample compartment cseeecccseeeecceeeeeeeeeeeeeseneeeseeeeesaeees 121 Adjusting the angle of reflection cccccccssseeeccceeeeeeeeceeeeeeesseaeeeeesseaeeeeseaas 121 Measuring with the reflectance attachment ccccccseeeeeeeeeeeeeeeeeeseeeeeens 121 Calculating the reflectante seitan 121 Calculating pathlength and refractive iNd X cccceeccecccceseeseeeeeeeeeeesaaeeeees 122 Care and maintenance arene eerie tee merece este tee ane ee tere rea ence eee emer eee ee 123 TECHNICA Cala cc O E a 123 integrating Sphere Tn se secces seceweeceseeee sees 125 D scriptionand ISO si oe a ce ae ae T 125 Design of
57. cell changer see Section Operation of the 8 cell changer p 44 Same as for the use of a single 8 cell changer the options slow time scan and the manual start of measurements are selectable for the combined use of two 8 cell changers 11 5 1 Staggered operation of two 8 cell changers for more than 8 samples In staggered operation with two cell changers up to 14 samples can be analyzed in one measurement series In this mode all samples are analyzed against the same reference Sample and reference beam path are interchanged by computer control so that samples can also be measured in the reference beam path Irrespective of this in the further description below the rear cell changer will always be referred to as cell changer in the reference beam path and the front cell changer as cell changer in the sample beam path In staggered operation the eighth cell position of the cell changer in the reference beam path and the first cell position of the cell changer in the sample beam path remain blank In the analysis first the cell changer in the sample beam path will drive to the first position and stay there while the cell changer in the reference beam path will successively move its cell positions into the beam When all samples of the cell changer in the reference beam path have been analyzed this cell changer will stop in its eighth position Afterwards the cell changer arranged in the sample beam path will successively move i
58. confirmed the 44 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 8 cell changer request You can use this option for kinetic measurements The measurement in the respective cell will then be started only after you added a starting substance Slow time scan Activate this option if in cyclic measurement mode you want to measure all samples on the cell changer successively first Deactivate the Slow time scan option if in cyclic measurements you want to measure all cycles of one sample first before the cell changer moves to the next position Interval Accessible only if the slow time scan option has been activated The interval time is the time from the beginning of a cycle to the beginning of the next cycle Hence it also includes the time required for sample measurement Enter the desired interval time in the textbox From the list box beside select the unit of time Pos 1 Cell changer moves to the first position Pos 1 Cell changer moves to the next position Adjustment Starts the adjustment of the cell changer Parking 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 11 4 2 Measurements with the 8 cell changer The measurement procedure with the 8 cell changer is analogous to that of the 6 cell changer Section
59. ct the temperature control unit and the heat exchanger see Sections Connection and operation of temperature control unit p 90 and Connection and operation of the heat exchanger p 94 Installing a second cell holder The second cell holder is installed largely in the way described above However the recess in the rear sample compartment wall is too small for allowing the electrical cables of two cell holders to be threaded through Therefore the accessory is supplied along with a different right angled bracket 1 Undo the right angled bracket mounted in the recess of the sample compartment In its place mount the supplied bracket Put the two supplied plastic foam strips into the recess 2 Install the second cell holder in the reference beam path 3 Lay the electrical cables as described above 4 Connect the cell holders to each other by means of a short piece of tube Connect one water tube each to every cell holder Establish the connections to the heat exchanger as described above 5 Connect the electrical cables to the temperature control units Inserting the cell 1 Turn the cover cap Fig 13 6 7 until the opposite grooves of the cover cap Fig 13 6 9 are in line with the lock screws Fig 13 6 8 2 Pull the cover cap upward and carefully put the cell into the block 3 Finally reattach the cover cap to the cell block Users Manual SPECORD 200 205 210 250 Accessories 07 2005 67 Analytik J
60. d in bottom position 2 0 eee cece cece ee eeeeeeeeeeeesaeeeeeeeeeeeeeaas 8 Ride Un iversal holder susreo aa aa E aaa a aE 11 Fig 2 2 Attaching and clamping the universal Nolder c ccseeeeeeeeeeeeeeeeeeeeeeeeeees 12 Fig o 1 100 mmceylindrical Cell nonr a a a i Tai 13 Fig 4 1 Solid Sample NOldelr ceecccccccccceeeseeeeeeeeeseeeeeeeeeeeeseeeeeeeeeeeeesaeeeeseeeeesaaas 15 Fig 4 2 Solid sample in holder Slide ccccccccccceceeeeeeeeeeeeeeceeeeeeeeeeeeeeaeeeeeeeeeeeeaaas 15 Fig 5 1 Holders for cylindrical Cells ict cence celta eatetee pel Sub enter ine bcteateieetuelnut aude 17 Fig 5 2 10mm thermocell Cylindrical cccccccsssecccseeeeeseeeeeseeeeeesseeeeseeeeeeseeessnees 17 Fig 6 1 Holder for round cells cso cin setae ites eceas eee aces recta Aten eaten aa 19 Fig 7 1 Holder for semi microcells cccccssseeeecceseeeeccaeeeeeeeeeeaeceeeeeeeeeessuegeeesseaaees 21 Fig 7 2 Holder for microcells adjustable with beam heights of 8 5 mm and 15 mm ee NS feo a Mecania ete eer a en eee ee 22 Fig 7 3 Holder for microcells adjustable c ccc cecceeeeseeeeeeeeeeeeeeeeeeeeeeeeseeneeeeenaaees 23 Fig 8 1 Thermostatted Cell holder ccccccceeeececceseeeecceeeseeesceeaeceessuaueeeeeeeagesesseeaess 25 Fig 8 2 Inserting the Magnetic stirrer COll ccccsecccccseeeeeseeeeceeeeeeseueeeeseneeeeneeeeesaees 26 Fig 9 1 Adjustable thermostatted Cell holder c
61. d the tubes through the provided tube ducts in the right hand sample compartment wall Fig 10 5 6 The tube ducts in the wall are provided with steps to achieve a higher light tightness 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 2 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 35 Analytik Jena AG 6 cell changer thermostatted 3 Thread the cable of the magnetic stirrer under the rear carrying rails and push it through between the two plastic foam strips in the recess in the sample compartment In doing so 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 4 Thread the cable through underneath the cover of the sample compartment Make sure the cable is not squeezed when the cover is closed 5 Connect the ribbon cable to the power supply Fig 10 3 7 by means of the adapter Fig 10 3 5 6 With the clamping lever pointing to the back place the 6 cell changer onto the front carrying rails Push the 6 cell changer to the right hand sample compartment wall as far as it will go Clamp it to the carrying rails by throwing the clamping lever to the
62. der 2 with its hook onto the rear of the two front carrying rails Slide it to the right hand wall of the sample compartment as far as it will go 2 Throw clamping lever 3 over to the right to clamp the universal holder 3 Slide holder 1 for cylindrical cells from top onto mounting plate 4 of the universal holder 4 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 13 Analytik Jena AG 100 mm cylindrical cell absorption tube 3 4 Care and transportation of cylindrical cell Store and carry the cylindrical cell only in the original packing Clean the cylindrical cell after every use 14 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Solid sample holder 4 Solid sample holder 4 1 Description and use The holder is suited for solids having a minimum diameter of 20 mm and a maximum pathlength of 25 mm The size of samples should not exceed 80 mm x 140 mm Guide Mechanical stop Spring clip Knurled screw Support block O AOON Fig 4 1 Solid sample holder 4 2 Using the holder and inserting the sample Sample Fig 4 2 Solid sample in holder slide 1 Slide the solid sample holder with its guide from top onto the mounting plate Fig 1 1 10 2 Loosen knurled sc
63. der to the temperature control unit see Section Connection and operation of temperature control unit p 90 Inserting the cell 1 Turn the cover cap Fig 13 2 9 until the opposite recesses Fig 13 2 8 are in line with the lock screws Fig 13 2 7 2 Pull the cover cap upward and carefully put the cell into the block 3 Finally reattach the cover cap to the cell block Cr Note Closing the cell block prevents the cell from being steamed up when working at temperatures below room temperature 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 59 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled Monitoring the cell internal temperature A Caution Fragile sensor Do not use force when attaching the sensor It is not necessary to press on the sensor as it receives sufficient pressure through the contact pins in the cover cap Caution Flashing temperature display If the temperature display Fig 13 17 2 and 3 on the temperature control unit is flashing either the cell sensor is not properly connected to the connector on the control unit or the sensor is defective 1 Close a standard cell with round stopper b
64. direction is wrong the pumping direction will be wrong too Use the tube adapter to interconnect pump tube and drain tube Insert the tube set in the sample holder 5 Plug the cell retaining spring onto the place that corresponds to the pathlength of the cell 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 Cassette sipper T Note After longer use it may happen that the pump tube section tensioned in the cassette sipper loosens its elasticity If the tube did not additionally become porous you can tension the second tube section between the middle and the third stopper in the tube cassette 14 3 2 Mounting the sipper in the sample compartment Wii Interface cable Drain tube Flow cell Sample aspirating tube AOUN Fig 14 3 Cassette sipper mounted in SPECORD 1 Thread the drain tube through one of the provided ducts Fig 1 1 6 or 11 in the sample compartment to the collecting bottle set up outside Lay the tube under the carrying rails so that it cannot jut into the beams when taking measurements The ducts in the sample compartment wall are provided with steps to increase the light tightness If the tube hooks to these steps when threading it through
65. ds with different data points Therefore enter the total measuring time here The entries in the Data Points text box will not be taken into account Instead enter the interval time on the Accessories tab Activate the Interval check box and enter the desired interval time If you fail to do so the measurements will be taken at the fastest possible cycle time until the end of the total measuring time 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 39 Analytik Jena AG 8 cell changer 11 8 cell changer D This cell changer is an automatic sample changing system The driving unit with stepper motor is controlled by WinASPECT software The cell changer has eight cell positions for holding 10 mm pathlength cells of the following outer dimensions 12 5 x 12 5 x 45 L x W x Hin mm The stepper motor drive of the driving unit conveys the cell holder within approx one second to the next position Together with a reflection coupler that defines the initial point of the motion range the stepper motor drive provides exactly reproducible alignment of the cells to the sample beam The 8 cell changer is optionally available with temperature control via an external ther mostat and or
66. e body in the SPECORD exactly in the same way as you did for the reference measurement 6 By taking two measurements with and without gloss trap you can determine the percentages of scattered and reflected radiation If you want to take very accurate diffuse reflectance measurements at a defined wavelength first calibrate the system using several certified standards same as in 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 19 6 Technical Data Spectral range Sphere material Sphere diameter Light entrance aperture Reflectance aperture Light exit aperture Dimensions L x W x H Weight Transmittance cells for liquid samples Solid samples for transmittance measurement L x W x H Samples for diffuse reflectance Sample holder for powder samples Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Integrating Sphere 380 1100 nm Spectralon 75 mm S 10 mm D 12 mm S 16 mm 150 mm x 105 mm x 145 mm 1 0 kg Width 12 5mm Pathlength up to 10 mm up to 250 mm x 85 mm x 15 mm Diameter up to 50 mm Depth up to 20 mm Diameter 16 mm Depth 5 mm 133 20 Figures Figures Fig 1 1 Sample comparnment esei E E E 7 Fig 1 2 Carrying rails mounte
67. e expansion of ice User s Manual SPECORD 200 205 210 250 Accessories 07 2005 55 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 13 1 2 Technical data of Peltier temperature controlled cell holder air cooled Guaranteed regulated temperature range at 25 C 10 60 C on models with Type A ambient temperature heat transfer 5 105 C on models with Type B heat transfer Overview 13 1 Technical data of Peltier temperature controlled cell holder Technical data of control unit Line fuses 2x T 2 5 A H 250V Type 19181 Wickmann EMC jamming and noise immunity acc to DIN The device may be installed and EN 61326 and 61326 A1 operated in all areas Fire resistance of the control unit case acc to HB 1 6 UL94 Relative humidity up to 90 at 30 C Overview 13 2 Other technical data of Peltier temperature controlled cell holder 56 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 13 1 3 Design of Peltier temperature controlled cell holder air cooled User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 12 9 14 8 6 4 1 2 3 1 Cell block with insulation 9 Cover cap 2 Cell with cell temperature sensor 10 Contact cap 3 Spacing
68. e of two 8 cell changers cccsssecccccseesececceeeseceeeeeeeeceeseuaeeeesseaneeessaaaneeess 45 Staggered operation of two 8 cell changers for more than 8 samples 46 Synchronous operation of two 8 cell ChANGErS ceeeeeeeeeeeeeeeeeeeeeeeaaees 47 CellicarQuSell cere ee ees eee eee 49 DESCrIPUOMIANG USE sas inarenedaiaentateaeanenaesamacdesaande 49 DESO eevee teem near ee eet VON NEe Mereret Mcetner preteen CaN ae Ma Cer mee en peer ar met Coe eee 49 Installation in Sample compartment cceeccecseeeeeceeeeeeeeeeeeeeeeeeesseeeeeseeeeeees 50 Operaia mete er ee eee enn te a a MEE te ee TE nee eee Eee 51 Peltier temperature controlled cell holders cell changers oera 53 Peltier temperature controlled cell holder air cooled cccccseeeeeeeeeeeeeees 54 sale MOLES eeen a a 55 Technical data of Peltier temperature controlled cell holder air cooled 56 Design of Peltier temperature controlled cell holder air cooled 04 57 Installation of Peltier temperature controlled cell holder in SPECORD 58 Se meer eee ner One ne rete ee nt ee Pe ere ee eer eer ee 60 Peltier temperature controlled cell holder with heat exchanget 06 62 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Contents 13 2 1 Safety notes for the use of the Peltier temperature controlled cell holder with FIG al OXCManG Cl ncdecvsressoaes Secs se rece
69. e rail stop 4 Cell block with insulation Fig 13 5 Bottom of Peltier temperature controlled 1x cell holder The part of the cell sensor immersing in the cell is made of Teflon and thus largely chemically resistant The upper part of the sensor consists of an anodized aluminum cap with an opening for the gold plated conductive tracks 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 61 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder with heat exchanger 13 2 13 2 1 62 Peltier temperature controlled cell holder with heat exchanger A sa The Peltier temperature controlled cell holder allows the temperature control of 10 mm pathlength cells of the following dimensions 12 5 x 12 5 x 45 46 L x W x H in mm Temperature control of the cell holder is performed by a separate control unit The rear side of the Peltier elements is cooled by a connected heat exchanger The sensor used for the control is a Pt100 measuring sensor located at the outer bottom corner of the cell block Beside the measuring sensor for temperature control two additional Pt100 sensors are used for the optional measurement of the temperature of the holder or the cell
70. e textbox From the list box beside select the unit of time Pos 1 Cell changer moves to the first position Pos 1 Cell changer moves to the next position Adjustment Starts the adjustment of the cell changer Parking 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 37 Analytik Jena AG 6 cell changer thermostatted 10 4 2 Measurements with the 6 cell changer Measurement without reference cell in cell changer 1 Place the reference cell onto the cell position in the beam path 2 Start the reference measurement by a click on the Reference toolbar button or by activating menu command Measurement Reference 3 Load the cell changer beginning with the position selected as First sample Place the other cells continuously onto the following cell positions up to the position defined as Last sample 4 Start the sample measurement with the corresponding Start Measurement toolbar butto or menu command Measurement Measurement Measurement with reference cell in cell changer 1 Place the cell containing the reference onto the position selected as First sample Place the other cells continuously onto the following cell positions up to the position defined as Laset sample 2 St
71. ecified on the rating plate at the rear panel of the devices Operation of the devices with any other operating voltage than that specified may result in their destruction Only use fuses of the specified type Section Technical data of Peltier temperature controlled 6 cell changer p 71 Do not operate the device in explosion risk rooms Type label and warning labels Observe the type label and the warning labels on the devices Accumulation of heat Make sure that you do not cover the ventilation slots in the bottom plate and on the rear panel of the device as well as on the front panel of the heat exchanger Heat accumulation might result in overheating and faults on the equipment Ingress of water Take care to ensure that no liquids can get into the control unit to avoid any damage to the device Do not place the heat exchanger or containers with liquids onto the control unit The control unit complies with the requirements of Protection Type IP 20 The PTC 600 PTC 601 Peltier temperature controlled 6 cell changer was produced and tested in compliance with the following standards and regulations e DIN EN 61010 1 IEC 1010 1 e 73 23 EC e 89 336 EC User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 13 3 3 Technical data of Peltier temperature controlled 6 cell changer O
72. ection The protection must not be made ineffective by the use of extension cables without earth conductor Caution Correct fusing Only use fuses of the specified type and rating gt Section Technical data of Peltier temperature controlled cell holder with heat exchanger p 64 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG gt gt gt Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder with heat exchanger Warning Do not operate the equipment in explosion risk rooms Warning Hot surface Before replacing any cells after operation at higher temperatures wait until they have cooled down sufficiently There is the risk of burns Caution Accumulation of heat Accumulation of heat might result in overheating and faults on the device Make sure that you do not cover the ventilation slots of the temperature control unit and of the heat exchanger Caution in handling liquids Take care to ensure that no liquids enter the temperature control unit to avoid any damage to the unit 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 63 Analytik Jena AG Peltier temperature controlled cell ho
73. ecularly as by the surface of a mirror To eliminate this portion insert the gloss trap Fig 19 1 19 in aperture Fig 19 1 11 after having removed locating pin Fig 19 1 12 Loading powder samples 6 J Eo L 5 A vy erik JTE ae Se F te D D i P 4 1 2 3 1 Retaining clip 5 Thrusting disk 2 Guiding pin 6 Knurled screw 3 Sample holder for powder samples 7 Integrating sphere 4 Cylindrical support for integrating sphere Fig 19 4 Integrating sphere with sample loading fixture Uncompressed powder samples must be loaded outside the SPECORD For that a special holding fixture Fig 19 4 is provided 8 Fill the sample into the holder for powder samples Fig 19 1 21 Slightly compress the sample and smooth the surface 9 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 131 Analytik Jena AG Integrating Sphere 10 Put the sample holder Fig 19 4 3 into the recess located at the underside Slightly clamp the sample holder by means of retaining clip Fig 19 4 1 by pushing down the clip on the guiding pin Fig 19 4 2 11 Carefully in
74. eeccceccsseeeceeeeeeeeeeeesaeeeeeeeaeeeeeeeeas 29 ig O22 APEG CEI oaia r a TA 29 Fig 10 1 Thermostatted cell holder and driving unit ccccecceeeeeeesseeeeeeeeeeeeeeeeeeas 32 Fig 10 2 Thermostatted cell holder with magnetic stirrer ccccceesseeeeeeeeeeeeeeeeees 32 Fig 10 3 Installation of magnetic stirrer nnnnennnnennnnennennnneernnesrrensrnnnsrrerserresrrenne 33 Fig 10 4 Cell holder with quick lock tube coupling ccceeeecccceeeeeeeeeeeeeeeeeseaeeeees 34 Fig 10 5 Installation Of Cell changer ccccseececcseeeeceseeeceeeecseeseecseeeeeseeseesseneeeens 35 Fig 10 6 Accessories tab Cell changer ccccccccssseeeeceeeeeeeeeeeeeeeeeeseeeaeeeeeeeesaaas 37 Fig 10 7 Cell changer Operating modes cccccccceecseeeeeeeeeeeeseeeseeeeeeeessaeaeeeeeeess 38 Fig 11 1 Transport lock on non temperature controlled 8 cell changer 41 Fig 11 2 BrCClIIGMANO SL eira a cereale los 42 Fig 12 1 Cell carousel Driving Unit ANd SAMI trAY cccceeeeeeeeeeseeeeeeeeeseeeeees 49 Fig 12 2 Cell carousel installed in sample CoMpartMent ccccceeeseeeeeeeseeeeeees 50 Fig 13 1 Peltier temperature controlled 1x cell holder with control unit 54 Fig 13 2 Peltier temperature controlled cell holder air cooled sseeeeeeeeeees 57 Fig 13 3 Installation of the PTC 100 in the sample compartment cccccce 58
75. eeeeseeeeeeeeesaaeeeeeeeas 115 Beam geometry in Absolute Reflectance Attachment ceeee 116 Reflectance attachment with large sample table cess 119 Mirror and small tablet pisses ieee tle Aiea laeeae 120 Optical path in reflectance attachment front view cccceeceeeeeeeeees 120 Example of interferences at an angle of reflection 60 00 122 Integrating sphere with accessory ItEMS ccceeeeeeeeeeeeeeeeeeeeeeeaeeeeeeeeas 126 Optical path in transmittance MEaSUreMENS cccccseeeeeeeeeeeeeeeeaeeeeees 128 Optical path in reflectance MEaSUrEMENS cccccceceeeseeeeeeeeeeesaeeeeees 130 Integrating sphere with sample loading fixture cceccceeeeeeeeeeeeeeeeeees 131 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG
76. emi microcells and microcells 24 insert it in the appropriate locating hole 7 Then screw it down again using knurled screw 2 Insert either an empty cell in the holder or a cell filled with solvent Leaf spring 5 will press the cell against cell guide 6 In the device driver menu command Measurement Set Parameters create a parameter record with e g the following measurement parameters Wavelength 500nm Integration time 0 1s Slit 2nm Correction No Cycle Mode Manual 20 Display Energy 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Thermostatted cell holder 8 Thermostatted cell holder 8 1 Description and use The thermostatted cell holder accommodates a 10mm pathlength cell of 12 5 x 12 5 x 45 L x W x H in mm with a minimum filling level of 25 mm You may optionally insert a magnetic stirrer in its bottom plate Temperature control is by an external fluid thermostat Observe the operating instructions provided with the thermostat The thermostatted cell holder is not suitable for the accommodation of HPLC cells gt Section Adjustable cell holder thermostatted p 29 You can place the thermostatted cell holder in the sample beam while working
77. ena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder with heat exchanger lt a Note Closing the cell block prevents the cell from being steamed up when working at temperatures below room temperature 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 Monitoring the cell internal temperature A Caution Fragile measuring sensor Do not use force when attaching the sensor It is not necessary to press on the sensor as it receives sufficient pressure through the contact pins in the cover cap Caution Flashing temperature display If the temperature display Fig 13 17 2 and 3 on the temperature control unit is flashing either the cell sensor is not properly connected to the corresponding connector ort he sensor is defective 1 Cell sensor 2 Cover cap of cell holder 1 2 Fig 13 7 Cell temperature measuring sensor PT100 1 Close a standard cell with round stopper by means of the supplied cell sensor 2 Put the cell into the cell block and close it by means of the cover cap the grooves are facing the lock screws 3 Lock the cover cap by slightly twisting it 4 On the temperature control unit switch the holder cell temperature selector to cell Extending the immersion depth of the measuring sensor 6
78. ent by the plastic foam strips supplied along with the accessory 4 Thread the electrical cables 2 to the back underneath the carrying rails Put the cables between the plastic foam strips in the rear sample compartment wall 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled SPECORD with recess underneath the sample compartment cover 5 Thread the cables through underneath the sample compartment cover and put the cable into the recess so that they are not squeezed when you close the cover SPECORD without recess underneath the sample compartment cover 5 Remove the knurled screws from the cover prop 5 Fold the cover backward Put the connecting plug of the electrical cables 2 through the slit between sample compartment cover and SPECORD basic device Screw on the cover prop again Remove the cover cap from the opening in the sample compartment cover 4 Put the electrical cable through the slit in the opening Slip the annular stopper over the electrical cables and insert it with the slit on top into the opening Fig 13 4 Fig 13 4 Sample compartment cover with cables threaded through 6 Connect the cell hol
79. eptacle for cells with turbid samples Mount for cell holder Duct for drain tube not visible Ducts for sample aspirating tubes sipper Sample 1 and reference beam 2 enter the sample compartment through the left hand wall The mounts for the cell holders 8 10 are arranged in front of the exit windows in the right hand sample compartment wall The two pairs of carrying rails serve to accommodate the accessories which easily clamp to the rods The receptacles for the cells 7 9 with turbid samples are located directly in front of the detector at the right hand sample compartment wall 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 Introduction Basics of SPECORD alignment The optical fibers of the measuring probe or the cables of the Peltier temperature controlled cell holder or the cell changer are threaded through the recess in the rear wall of the sample compartment 5 The three ducts 6 11 in the right hand sample compartment wall are used for threading through the sample drain tube and the coolant tubes for the thermostat The ducts in the front side of the device cover 12 are provided for threading through the aspirating tubes of the sipper system 1 3 2 Adjustment of zeroth order In zeroth
80. er prop again Remove the cover cap from the opening in the sample compartment cover 2 Put the electrical cable through the slit in the opening Slip the annular stopper over the electrical cables and insert it with the slit on top into the opening Fig 13 4 p 59 7 Lay the thermostatting tubes underneath the rear carrying rails Thread them through the provided ducts in the right hand sample compartment wall The tube ducts are provided with steps to achieve a higher light tightness 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 Connect the tubes to the thermostat We recommend using quick lock couplings that allow drip free connection and disconnection of the thermostat 8 Connect the cell changer to the temperature control unit gt Section Connection and operation of temperature control unit p 90 9 Connect the heat exchanger Section Connection and operation of the heat exchanger p 94 Installing a second cell changer A Caution Correct cable connections in sample compartment Connect the cell changer installed in the rear reference beam path to the right connector in the sample compartment Connect the cell changer installed in the front sample beam path to the left connector The second Peltier temperature controlled 8 cell changer is installed largely in the way desc
81. erating voltage of the power supply unit 7 agrees with the available line voltage The driving unit may optionally be fitted with a stirrer containing two magnets One magnet is located underneath the measuring place the other one underneath the place before the measuring position The magnetic stirrers are to be mounted outside the sample compartment 1 Lift the cell holder off the driving unit 2 Putthe carrier Fig 10 3 1 for the stirrer coils onto the provided place Fig 10 2 and fasten it by means of the screws from the bottom 3 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 4 Reattach the cell holder to its support on the driving unit User s Manual SPECORD 200 205 210 250 Accessories 07 2005 33 Analytik Jena AG 6 cell changer thermostatted 5 Put the stirring magnets Fig 10 3 1 into the cells 6 Connect the power supply Fig 10 3 7 to a power outlet and turn the speed control knob Fig 10 3 8 to adjust the stirring speed The magnetic stirrer is operating 10 3 2 Connection to a thermostat 1 3 4 1 Thermostatting tube 3 Female tube connector 2 Male tube connector 4 Locking lever Fig 10 4 Cell holder with quick lock tube coupling The cell holder is connected to an external fluid thermostat through tubes with quick lock couplings The cell holder is p
82. ete ei a nie eee Wer enor Ter ete ene eee Veen eer er 19 6 3 Using the holder for round Cells iriiria a EA 19 7 Holder for semi microcells and microcells 21 7 1 B scnpion and USEd siss aban eet N EE E E A a ai 21 7 2 Hold r Ttor semi MICKOCSNS scsrorrnai a A meena 21 7 3 Adjustable holder for microcells non thermostatted 8 5 mm 15 mm beam ALERT E PEE E EE E AE E A E N N EAE E E E old SE 22 7 4 Adjustable holder for microcells non thermostatted 8 5 mm beam height 23 8 Thermostatted cell Nolde r ccccesceseseeeeeeeeeeeeeeneees 25 8 1 D scription and USec ara aaa a aa a raia eaaa S 25 8 2 JOS CHOU OM ane a eats eeceaneten lames esate 25 8 3 Using the thermostatted Cell holder ccccccsseeecccceeeeeeeeeeeeeeeeeseeeeeeeessaeeeess 25 8 3 1 Connection and installation in sample compartment ccccseeeeeeeeeeeeeeeees 25 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 1 Analytik Jena AG Contents 8 3 2 9 1 9 2 10 10 1 10 2 10 3 10 3 1 10 3 2 10 3 3 10 4 10 4 1 10 4 2 10 4 3 11 11 1 11 2 11 3 11 4 11 4 1 11 4 2 11 5 11 5 1 11 5 2 12 12 1 12 2 12 3 12 4 13 13 1 13 1 1 13 1 2 13 1 3 13 1 4 13 1 5 13 2 Inserting the magnetic stirrer ccccssececceececceeeecceeececceseecsaeeeesseeeessaneeeseaes 26 Adjustable cell holder thermostatted 0 29 MserningIhe telesis nea aa e a e 30 Aligning the cel srein aE
83. ew obscured Screws for horizontal adjustment 2nd screw obscured Top part of adjustable cell holder Lever 29 Adjustable cell holder thermostatted 9 1 Inserting the cell Unscrew three screws 1 and remove lid 2 Insert the cell and screw down lid 2 again Put the adjustable cell holder onto the two front carrying rails of the sample compartment Fig 1 1 1 Push it to the right as far as it will go and clamp it by throwing over lever 8 to the left 9 2 Aligning the cell For rough orientation it is advisable to observe the passage of the sample beam through the cell 1 Adjust the zeroth order of the monochromator grating as described in Section Adjustment of zeroth order p 8 In this mode undispersed white light is passing through the sample compartment which can be observed very well You can check the illumination of the cell by means of a white screen e g a strip of paper Align the cell so that the sample beam is centered on the aperture of the cell Fine adjustment is done by taking an energy measurement 3 30 In the device driver menu command Measurement Set Parameters create a parameter record with e g the following parameters Wavelength 500nm Integration time O 1s Slit 2nm Correction No Cycle Mode Manual 20 Display Energy Loosen the four screws that fix the cell holder in position 5 until the top part of the adjustable cell holder 7 can be moved
84. he heat exchanger p 94 Adjustment of the Peltier temperature controlled 6 cell changer The cell changer can be adjusted computer controlled to optimally position the cells in the beam Adjustment is necessary e At the first use of the cell changer e After wavelength calibration e After relocation of the SPECORD e When working with microcells 1 Install the empty cell changer in the sample compartment 2 Onthe Accessories tab of the measurement parameter window activate the 6 cell changer Peltier option 3 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 75 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 76 If you intend to use microcells in the analyses insert a microcell filled with water in every of the six cell positions 4 Start automatic adjustment by a click on the Adjustment button Monitoring the cell internal temperature PE A 1 Cell changer 2 Connector for cell sensor 3 Cell sensor 4 Storage receptacle for connector Fig 13 11 Cell measuring sensor for the Peltier temperature controlled 6 cell changer 1 Close a standard cell with round stopper with the supplied cell measuring sensor Fig 13 11 3 in place of the standard stopper 2
85. he sample Raps resulting from this is R abs a JR In the graph and in the result table Raps is presented in percent 17 7 Care and maintenance A Caution Contamination of reflectance attachment Take care not to damage the mirrors by contamination Observe the instructions on the care of mirrors e Keep all mirrors of the reflectance attachment free of dust and grease Don t touch mirror surfaces with bare fingers e Remove dust particles on mirrors using a soft clean and grease free brush e Carefully wipe off traces of grease from mirrors using a cotton swab soaked with distilled water and curd soap Don t exert any pressure in wiping Then wipe with a new cotton swab soaked with distilled water only Finally dab metal mounts dry e Carry and store the absolute reflectance attachment only in a closed box 118 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Variable Angle Reflectance Attachment 18 Variable Angle Reflectance Attachment 18 1 Description and use With this accessory you can determine pathlength and refractive index of solid samples This is done by measuring the reflectance at different angles of reflection over a defined wavelength range For the determination of pathlength the interferences that occur during the measurement are utilized by evaluating the number of interference maxima appearing in the defined wavelength region Prior to sample measurement you mu
86. hen running analyses at low temperatures 13 3 6 Settings in WinASPECT software The cell changer is controlled by WinASPECT software On the Accessories tab of the measurement parameter window choose the 6 cell changer Peltier option Cell changer First sampe gt _ _ _ _ Na Pos 1 Last sample ml Ho 6 Pos 1 Tat sample Reference z Manual Start I Adjustment Slow time scan Parking Fig 13 12 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 77 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 1 sample Reference Start manually Slow time scan Pos 1 Pos 1 Adjustment Parking 13 3 7 Measurement procedure 78 The sample placed on the 1 position selected above is treated as reference In this case it is not necessary to run the reference measurement separately The reference measurement will be performed within the normal sample measurements 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 measurement
87. ier temperature controlled cell holders cell changers Peltier temperature controlled cell holder with heat exchanger Technical data of heat exchanger WC 600 WC 601 Weight without coolant Dimensions W x H x T Line voltage Line frequency Power consumption Line fuses for WC601 Line fuses for WC601 EMC jamming and noise immunity as per DIN EN 61326 and 61326 A1 Fire resistance of the case of the heat exchanger according to UL94 Protection Type Coolant Maximum delivery head Operating temperature range Transport and storage temperature range Relative humidity 3 2 kg 225 x 175 x 200 mm 220 240 V 50 Hz 50 VA 2x T 0 5 A H 250V Type 19181 Wickmann 2x T 1 6 A H 250V Type 19181 Wickmann The device can be installed and operated in all environments HB 1 6 IP 20 Approximately 0 4 distilled water with an addition of 4 ml isopropanol 1 2m 15 C 2 435 6 40 C 460 C up to 90 at 30 C Overview 13 5 Technical data of heat exchanger for PTC 600 PTC 601 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 65 Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder with heat exchanger 13 2 3 Design of Peltier temperature controlled cell holder with heat exchanger Connector for connection to heat exchanger 5 pole and 9 pole connector for connection to temperature control unit Clam
88. integrating sphere ccccseececceeeeeceeseecceseecceueeeseeneeesseseesseaeees 126 Measurements with the integrating SPNELPE ccecccecseeeeeseeeeeeeeeeeeseeeeeees 127 Transmittance measurements ccceceeceeeeeeeeceeeeeeeeeeaaeeeeeseaueeeesseaeeeeenas 127 Reflectance MEASUlEMOINS xisscasessdexventedeseciccstxweseeiebvenccdevesa tides edeexcerneseebeeeese 129 TCIM AND Atay na a a enc 133 PLCS eee creda cecetecenecetevececamacencctine E EEN 135 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Analytik Jena AG Introduction Safety notes 1 Introduction This manual contains the description of the following devices e SPECORD 200 from S N 222 U or V W X 100 e SPECORD 205 e SPECORD 210 e SPECORD 250 If the descriptions equally refer to all three models only the collective term SPECORD will be used In this manual the following symbols are used to refer you to warnings and notes A Danger Danger messages must be strictly observed to prevent personal injury Caution Caution messages refer you to procedures which if not observed could result in damage to the equipment A Warning Dangerous electric voltage AN Warning Emission of UV radiation gt Disconnect power cable a Note This note must be followed to obtain correct measurement results For easier navigation within the manual the manual uses the following system e Chapters and illustrations are
89. ion to heat exchanger S600 clamping lever CON OOF WD Fig 13 13 Design of Peltier temperature controlled 8 cell changer User s Manual SPECORD 200 205 210 250 Accessories 07 2005 83 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 13 4 4 Installation of Peltier temperature controlled 8 cell changer 84 Cover prop Opening with slit in sample compartment cover Connection cables to temperature control unit Recess in rear sample compartment wall Connector to SPECORD Water connection tubes to heat exchanger Clamping lever Cell block with insulation CON OOoBRWDNDN Fig 13 2 Installation of Peltier temperature controlled 8 cell changer Lay connection cables tension free The connecting cables and the coolant tubes must be laid without tension and in a way that they do not hinder the movement of the cell changer while in operation Make sure that the electric cables are not tensioned and the coolant tubes are not folded Take care to ensure that the coolant tubes and the connecting cables do not project into the light path of the sample or reference beam path 1 Replace the plastic foam stopper in the recess in the rear sample compartment wall 4 by the two plastic foam strips supplied along with the accessory 2 Remove the carrying rails from their top position and mount them in their bottom position Section
90. l SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Cell carousel 12 Cell carousel 12 1 Description and use The cell carousel is an automatic sample changing system connected to and controlled by the SPECORD It consists of two separable modules e acell holder e a driving unit with stepper motor The cell carousel contains 15 places for 10 mm pathlength cells of the following outer dimensions 12 5 x 12 5 x 45 Lx W x Hin mm 12 2 Design 1 Driving unit 6 Knurled screw 2 Tray support with guiding slot 7 Clamping lever 3 Sample tray 8 Stop bolt 4 Cell holder 9 Connection cable to SPECORD 5 Handle Fig 12 1 Cell carousel Driving unit and sample tray User s Manual SPECORD 200 205 210 250 Accessories 07 2005 49 Analytik Jena AG Cell carousel 12 3 50 Installation in sample compartment Fig 12 2 Cell carousel installed in sample compartment 1 First mount the carrying rails in the sample compartment in their bottom positions Section Changing the position of the carrying rails p 8 With clamping lever Fig 12 1 7 facing the rear side place the driving unit Fig 12 1 1 of the cell carousel onto the two front remounted carrying rails in the sample compartment Push the driving unit to the right hand sample compartment wall so that the stop bolt touches the right hand wall Fasten the driving unit to the carrying rails by throwing the clamping lever down left as f
91. larly mirror 3 Fig 19 1 7 For that only use dry dust free and oil free compressed air or nitrogen You may also clean the Spectralon locating surfaces For that use dry and clean compressed air then rinse the surfaces with distilled water and finally blow them dry To remove sticky dirt from these surfaces you may also use fine grained abrasive paper 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 125 Analytik Jena AG Integrating Sphere 19 2 Design of integrating sphere 7 8 9 18 6 10 verdeckt 5 4 3 2 1 Retaining clip 1 for reflectance sample 12 Knurled locating pin 2 Guide pin for retaining clip 1 13 Aperture to detector angle 3 Mirror 1 14 Locating surface 1 for horizontal mounting 4 Adjustable stop for cells 15 Locating surface for vertical mounting 5 Handle for retaining clip 16 Locating surface 2 for horizontal mounting 6 Mirror 2 17 Aperture for reflectance measurements 7 Mirror 3 18 Spectralon insert in place of gloss trap 8 Retaining clip 2 for transmission samples 19 Gloss trap 9 Guide for cells 20 Reflector 10 Aperture for transmittance measurements 21 Holder for powdery samples 11 Aperture for gloss trap 22 Spectralon insert for reflectance aperture Fig 19 1 Integrating sphere with accessory items The
92. lders cell changers Peltier temperature controlled cell holder with heat exchanger 13 2 2 Technical data of Peltier temperature controlled cell holder with heat exchanger Principle Thermoelectric heating and cooling Cooing at rear panel of TEC Water cooled by connection of an external thermostat Guaranteed regulated temperature 10 15 C range at 25 C ambient temperature Block temperature adjusting range 20 105 C Setting accuracy 0 1 degree Reading accuracy 0 1 degree Regulating accuracy 0 1 degree Overview 13 3 Technical data of Peltier temperature controlled cell holder with heat exchanger Technical data of control unit Weight of control unit 2 5 kg Dimensions B x H x T 225 x 130 x 200 mm Line voltage 100 240 V Line frequency 50 60 Hz Power consumption 75 VA Line fuses 2 x T 2 5 A H 250V Type 19181 Wickmann EMC jamming and noise immunity The device may be installed and operated in all acc to DIN EN 61326 and 61326 A1 environments Fire resistance of the control unit acc HB 1 6 to UL94 Enclosure Protection 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 64 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Pelt
93. lectance measurements of textured rough grained etc surfaces such as cellulose leather or fabrics and of samples with azimuthal gloss i e a gloss that varies while rotating the sample about its surface normal Fig 19 3 illustrates the optical path in reflectance measurements 4 2 10 8 7 6 1 Mirror 2 6 Spectralon insert for reflectance aperture 2 Mirror 3 7 Reflectance aperture for reflecting powder sample 3 Gloss trap 8 Diffuse reflectance 4 Reflector 9 Mirror 1 5 Detector 10 Optical path of SPECORD Fig 19 3 Optical path in reflectance measurements Preparing the measurements 5 First insert reflector Fig 19 1 20 as far as it will go into the round aperture in the middle of the rear mount for the cell holder The flange of the reflector should rest on the mount 6 You can take reflectance measurements of solid and powder samples For the measurement of solid samples it is advisable to insert the sohere body in such a way that the carrier of mirrors 2 and 3 Fig 19 1 6 and 7 points to the back and aperture 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 Integrating Sphere 7 The samples do not always scatter back 100 of the incident radiation a significant portion is also reflected sp
94. length of the sample using the following formula A2 Ai m 2 A2 A1 Jn sin A ho gt rhi d Thickness of sample m Number of interference maxima after zeroth order maximum see Example n Refractive index of sample Adjusted angle of reflection Ai Wavelength of zeroth interference maximum A2 Wavelength of m interference maximum Wavelengths A and A2 must be determined as accurately as possible For that in WinASPECT software use the Peaklist function of the Data Handling menu Example Measuring curve 100 0 90 0 80 0 70 0 60 0 50 0 40 0 30 0 20 0 10 0 0 60 330 0 400 440 480 520 560 600 640 680 720 760 800 440 892 5 Ax A gt Fig 18 4 Example of interferences at an angle of reflection 60 122 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Variable Angle Reflectance Attachment The curve shown above has been scanned at an angle of reflection of 60 It contains maxima of zeroth to fourth order 18 8 Care and maintenance A Caution Contamination of reflectance attachment Take care not to damage the mirrors by contamination Observe the instructions on the care of mirrors e Keep all mirrors of the reflectance attachment free of dust and grease Don t touch mirror surfaces with bare fingers e Remove dust particles on mirrors using a soft clean and grease free brush e Carefully wipe off traces of grease from mirrors using a
95. ls Wavelength 500nm Integration time 0 1s Slit 2nm Correction No Cycle Mode Manual 20 Display Energy 4 Align the cell holder at right angles to the beam path by taking repeated measurements and turning knurled screw 6 each to shift the cell mount until you obtain the maximum energy 5 Turn screw 4 to adjust the cell holder vertically until you obtain maximum energy 7 4 Adjustable holder for microcells non thermostatted 8 5 mm beam height 1 Fastening screw 2 Knurled screw for fastening the rider 3 Rider 4 Knurled screw for horizontal adjustment 5 Leaf springs 6 Cell guide 7 Locating holes Fig 7 3 Holder for microcells adjustable Technical Data Pathlengths of microcell 1 2 5 10 mm Height of beam center 8 5 mm Width of cell 12 5 mm Inserting the holder 1 Slightly unscrew knurled screw 1 on the holder to avoid jamming when you insert the holder 2 Slip this holder onto the mount for cells or the universal holder and push it down as far as it will go The universal holder must be moved as far as possible to the right hand wall of the sample compartment Tighten knurled screw 1 to fix the holder in the optical path of the SPECORD 4 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 23 Analytik Jena AG Holder for s
96. lysis of such samples use vapor tight stoppered cells Observe specific instructions 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 1 2 Care of accessories The accessories are largely maintenance free The following rules apply to all accessories Introduction Care of accessories M Avoid any contamination by handling sample substances carefully E Wipe off spilt samples or reagents immediately with an absorbent cloth or cleaning tissue E Do not expose accessories to corrosive atmospheres to prevent corrosion If provided observe the additional instructions on the care of individual accessory units 1 3 Basics of SPECORD alignment 1 3 1 Sample compartment of SPECORD 5 6 4 2 3 3 4 8 5 2 9 6 10 8 1 a 9 10 11 12 Fig 1 1 Sample compartment Sample beam path with two carrying rails Reference beam path with two carrying rails Connector for sipper and cell changer Connector reserve Stopper for duct of optical fiber of measuring probe or electrical cables Duct for coolant tubes Receptacle for cells with turbid samples Mount for cell holder Rec
97. m the sample compartment and sends it into the optical fiber 2 The optical fiber transmits the light to the measuring probe 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 113 Analytik Jena AG Fiber coupling for measuring probes A Caution Extraneous light Like with all other measurements too take care that no extraneous light enters the sample compartment For that it is necessary to make sure that the measuring probe does not capture any extraneous light Among others use the facilities for shielding extraneous light provided by the probe manufacturer 16 3 Design and function of the fiber coupling with SMA connectors In this case the adapter Fig 16 1 1 contains two optical fibers that are equipped with SMA connectors each 16 4 Installation of the adapter in the sample compartment A Caution Do not squeeze the optical fibers When you close the sample compartment cover take care that the optical fibers are not squeezed 1 Slide the adapter holder onto the cell holder mount of the sample beam in the sample compartment wall Fig 1 1 10 2 Put the adapter through at the back underneath the sample compartment cover Remove the lid from the rear circular opening of the sample compartment cover From the
98. measurement by a click on the corresponding button on the WinASPECT desktop Then follow the procedure described below under Sample measurement Sample measurement Without additional wash steps m Hold the sample to be analyzed to the aspirating tube E Start the measurement by a click on the Measurement start button The sample is being aspirated and the measurement started With activated Wash before measurement option m On the WinASPECT desktop click on the measurement start button This will bring up a message window prompting you to hold the wash vessel to the aspirating tube E Bring the wash solution to the aspirating tube m Start the wash process with OK When the wash process is finished a message window appears prompting you to prepare the sample to be analyzed m Bring the sample to the aspirating tube E Start the measurement with OK The sample is being aspirated and the measurement started With activated Wash after measurement option E Bring the sample to be analyzed to the aspirating tube E Start the measurement by a click on the measurement start button The sample is being aspirated and the measurement started When the measurement process is finished a message window appears prompting you to prepare the wash solution E Bring the wash solution to the aspirating tube m Start the wash process with OK 102 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG
99. mum of 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 79 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 13 4 1 Safety notes 80 A gt e gt Electric shock The temperature control unit and the heat exchanger are electrically powered At several parts inside the system extremely hazardous electrical voltages are accessible To ensure Protection Class protective earth connection of the device connect the power plug of the device only to a power outlet with protective earth conductor Connect control unit heat exchanger and SPECORD to the same phase of the line power supply e g to a multiple socket power outlet Before connecting the devices to the power outlet make sure the line voltage supplied agrees with the operating voltage specified on the rating plate at the rear panel of the devices Operation of the devices with any other operating voltage than that specified may result in their destruction Only use fuses of the specified type gt Section Technical data of Peltier temperature controlled 8 cell changer p 81 Disconnect the power cable before replacing any fuses Do not operate the device in explosion risk rooms Type label
100. na AG Peltier temperature controlled cell holders cell changers Connection and operation of temperature control unit 13 5 Connection and operation of temperature control unit 13 5 1 Connecting the temperature control unit 1 2 3 4 5 9 pole and 15 pole connectors RS232 port Power input connector Fuse holder for line fuse Power switch Type label oor ON Fig 13 16 Back panel of temperature control unit 1 Connect the 9 pole and the 15 pole connectors of the cell holder cell changer to the corresponding connectors Fig 13 16 1 on the back panel of the temperature control unit 2 Connect the power cable to the power input connector Fig 13 16 3 and then to a power outlet 90 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Connection and operation of temperature control unit 13 5 2 Settings on temperature control unit 1 4 5 auseed CTRON 08 8 CP y 3 l g f _ vy Ei ov 10 ae 6 7 1 Control module 2 Block temperature display 3 Temperature display of holder cell 4 Decrement button 5 Increment button 6 PGM button 7 EXIT button 8 Speed control for stirring magnets only for cell holders cell changers with magnetic stirrer 9 Holder cell temperature selector switch 10 Status lamp for heat exchanger not used on air cooled Peltier temperature controlled cell holders Fig
101. nstall the sphere body either with the carrier of mirrors 2 and 3 Fig 19 1 6 and 7 pointing upward vertical installation or with the carriers of the two mirrors rotated by 90 and pointing to the front side of the instrument horizontal installation Position for the measurement of liquid samples in cells Install the sohere body with the carrier of the two mirrors rotated by 90 and pointing to the front side of the instrument horizontal installation Transmittance measurement procedure 1 Inthe Device Driver dialog of WinASPECT software create the desired measurement parameter record Choose the following accessory specific options for the transmittance measurement Measurement parameter Option to be activated Correction Reference Slit As wide as possible to obtain a high energy level 2 Insert the two Spectralon inserts for the gloss trap Fig 19 1 18 and the reflectance aperture Fig 19 1 22 in the sphere body 3 Carry out the reference measurement For that you may insert a standard 4 Insert the sample and fix it by means of retaining clip 2 Fig 19 1 8 by moving it towards the sample with the handle Fig 19 1 5 until it is slightly clamped Make sure to install the sohere body in the SPECORD exactly in the same way as you did for the reference measurement Then carry out the sample measurement If you want to take very accurate transmittance measurements at a defined wavelength first calib
102. ol unit of the magnetic stirrer to the power outlet Thread the thermostat tubes through underneath the rear carrying rails Thread the tubes through the provided ducts in the right hand sample compartment wall 4 The ducts in the sample compartment wall are provided with steps to increase the light tightness If the tube hooks to these steps when threading it through try to release it by slightly turning it When it becomes already visible at the other end of the duct bend it to the opening e g by means of a pen Connect the tubes to a thermostat We recommend using quick lock couplings that allow drip free connection and disconnection of the thermostat Put the cell changer with the clamping lever facing the back onto the relocated carrying rails 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 43 Analytik Jena AG 8 cell changer 5 Thread the interface cable to the back underneath the rear carrying rails and connect the plug to the left connector on the back wall of the sample compartment Adjustment of the cell changer The cell changer can be adjusted computer controlled to optimally position the cells in the beam Adjustment is necessary e At the first use of the cell changer e After wavelength calibration e After relocation of the SPECORD
103. on 1 7 Fig 7 2 Holder for microcells adjustable with beam heights of 8 5 mm and 15 mm adjustable Technical Data Pathlengths of microcell up to 10 mm Height of beam center 8 5 and 15 mm Outside cell dimensions 12 5 x 12 6 x 45 mm Installing the cell holder in the SPECORD The cell holder contains a 6 5 mm high insert which is to be inserted in an opening below the cell when using cells of 8 5 mm beam height 1 To insert a cell pull out handle 1 a little bit and insert the cell from top Shift thrust pad 5 if necessary by turning knurled screw 6 2 From top slide down holder 3 onto the mount for cells Fig 1 1 10 as far as it will go Alignment of cell When you use the holder for the first time or when it is misaligned it is advisable to realign the cell to the beam path First look at the passage of undispersed white light through the cell 1 Adjust zeroth order in the beam path Section Adjustment of zeroth order p 8 2 Look through the slit 7 to see how the light is incident on the cell aperture Turn knurled screw 6 until the light appears centered on the cell aperture Fine adjustment is done by taking an energy measurement 3 Inthe device driver menu command Measurement Set Parameters create a parameter record with e g the following parameters 22 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Holder for semi microcells and microcel
104. on to be activated Correction Reference Display Reflectance Wavelength range Sufficiently large to get a sufficient number of interference maxima if you intend to carry out a layer thickness measurement Accessory Reflectance variable 2 Place the provided reference mirror onto the tabletop 3 and clamp it with the sample holding clips 4 Carry out the reference measurement with this mirror 3 Replace the reference mirror by the sample to be measured Carry out the sample measurement 18 6 Calculating the reflectance The measured reflectance R is calculated from the sample measurement reference measurement ratio r Rsample Sample measured in W configuration R 2 Sample r fReference Reference measurement in V Reference configuration L IRs Intensity after reflection at the Terin reference mirror reference beam te lReferenc beam Intensity in reference beam path User s Manual SPECORD 200 205 210 250 Accessories 07 2005 121 Analytik Jena AG Variable Angle Reflectance Attachment bz lps Intensity after the reflection at the lme 7 sample I Reference beam The result of the measurement is the relative reflectance of the sample relative to the reference mirror Rra lpg Rrel R RS In the graph and in the result table Rrei is presented in percent 18 7 Calculating pathlength and refractive index If the refractive index of the sample is know you can calculate the path
105. or may project into the sample beam thus distorting the measurement results The stepper motor drive of the driving unit moves the cell holder to the next sampling place within approximately 1 second In combination with a reflected light optocoupler which defines the starting point of the motion range the stepper drive ensures exactly reproducible alignment of the cells to the measuring beam SPECORD 2 1 1 Temperature control unit with status indicator for heat exchanger 2 Heat exchanger 3 Peltier temperature controlled 6 cell changer Fig 13 8 Peltier temperature controlled 6 cell changer with SPECORD 210 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 69 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 13 3 2 Safety notes 70 A Electric shock The temperature control unit and the heat exchanger are electrically powered At several parts inside the system extremely hazardous electrical voltages are accessible To ensure Protection Class protective earth connection of the device connect the power plug of the device only to a power outlet with protective earth conductor Connect control unit heat exchanger and SPECORD to the same phase of the line power supply e g to a multiple socket power outlet Before connecting the devices to the power outlet make sure the line voltage supplied agrees with the operating voltage sp
106. or this R Reference S Sample 0 Blank cell position Taking measurements in staggered operation In staggered operation the reference measurement can be performed in one of the following ways 1 The reference is not measured separately before taking sample measurements but in the sample measurement process The first cell position on the cell changer holds the reference cell In the measurement parameters on the Accessories tab activate the 1 sample reference option 2 The reference is measured before samples are analyzed In the measurement parameters on the General tab activate the Reference option and on the Accessories tab the 1 sample reference option For the reference measurement place the reference cell in the sample beam path and keep the reference beam path blank 3 Measurements with strongly absorbing reference In the case of strongly absorbing references it is useful to use the reference to additionally attenuate the reference signal for sample measurements and to create a balanced energy ratio between reference and sample beam path In the measurement parameters on the General tab activate the Reference option and on the Accessories tab deactivate the 1 sample reference option The reference measurement is taken with blank sample and reference beam paths For the sample analysis place a reference cell each on the eighth position in the reference beam path and on the first position in the sample beam path
107. owing options for the use of the sipper Sipper Purnp time 1 00 Pump ON T Wash before measurement Wash after measurement Fig 14 4 Device driver Accessories tab with selected Sipper option For the control of the sipper via WinASPECT the following options are available Option Button Description Pump time s The pump time is the time needed to optimally transfer the sample into the cell Because of the rinse effect approximately 2 3 of the sample should flow through the cell and 1 3 of the sample be before the cell Adjusting range 0 300s Wash before Performs a wash step before sample measurement measurement The wash time is 1 5 x Pump time At the end of the entry procedure the time will be rounded by software to tenths of a second Wash after measurement Performs an additional wash step after sample measurement Pump ON OFF 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 101 Analytik Jena AG Cassette sipper 14 4 2 Performing a sample measurement Reference measurement If this Measurement parameter option was selected in the device driver take a reference measurement Feed the sample as described in the Section Sample measurement below m Start the reference
108. p Move the tube holder 12 down as far as it will go Push the sample tube down until it is about 1 2 mm above the bottom of the cup When using a magnetic stirrer put the stirrer magnet first into the cup Adjust the immersion depth so that the MFA tube does not touch the magnet Make sure that the black guide tube does not immerse in the sample If the guide tube immerses in the sample push it up Then move down the MFA tube within the guide tube until its end is again about 1 2 mm above the bottom of the cup or the stirrer magnet Tighten the knurled screw 11 on the tube holder 12 Switching on the XYZ autosampler A Caution Correct order of switch on Make sure to follow the above order in switching on the system to ensure that the autosampler is moved to the correct starting position If you should have switched off the autosampler in the mean time restart the software once more after switching on the autosampler Switch on autosampler and SPECORD in the following order 1 Switch on autosampler 18 Fig 15 2 2 Switch on PC and SPECORD 3 Start WinASPECT software and initialize the SPECORD 4 Activate the device driver measurement parameter dialog box User s Manual SPECORD 200 205 210 250 Accessories 07 2005 109 Analytik Jena AG APG 53 100 XYZ Autosampler 15 5 Sample measurement In the Device Driver choose the following accessory specific measurement parameters 1 In WinASPEC
109. perating principle Thermoelectric heating and cooling Cooling of rear panel of TEC Water cooled Guaranteed regulated temperature range at 25 C ambient temperature PTC 600 with heat exchanger WC 600 10 C 60 C PTC 601 with heat exchanger WC 601 5 C 4 105 C Block temperature setting range PTC 600 with heat exchanger WC 600 5 C 65 C PTC 601 with heat exchanger WC 601 20 C 105 C Setting accuracy 0 1 degree Reading accuracy 0 1 degree Regulating accuracy 0 1 degree Overview 13 6 Technical data of PTC 600 PTC 601 Technical data of control unit Weight 2 5 kg Dimensions W x H x T 225 x 130 x 200 mm Line voltage 100 240 V Line frequency 50 60 Hz Power consumption 150 VA Line fuses 2 x T 2 5 A H 250V Type 19181 Wickmann The device can be installed and operated in all environments EMC jamming and noise immunity as per DIN EN 61326 and 61326 A1 Fire resistance of the case of the control unit HB 1 6 according to UL94 Protection Type IP 20 Data interface RS232 port Operating temperature range 15 C 35 C Transport and storage temperature range 40 C 60 C Relative humidity up to 90 at 30 C Analytik Jena AG Overview 13 7 Technical data of control device for PTC 600 PTC 601 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 71 Peltier temperature controlled cell holders cell changers
110. pin 11 Lock screw for contact cap 4 Connectors for connection to the 12 Heat transfer device control device 13 Heat exchanger housing with 5 Right guide rail stop intake slots 6 Quartz window 14 Clamping lever 7 Lock screws 15 Pressure plate 8 Recess Fig 13 2 Peltier temperature controlled cell holder air cooled 57 Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 13 1 4 Installation of Peltier temperature controlled cell holder in SPECORD 58 i y f i _ _ me 1 Clamping lever 2 Electrical cables to temperature control unit 3 Recess with plastic foam stopper 4 Hole with slot in sample compartment cover 5 Knurled screws for fastening the cover prop Fig 13 3 Installation of the PTC 100 in the sample compartment 1 The air cooling juts out through an opening in the sample compartment cover Remove the knurled nuts from the sample compartment cover and remove the cover that closes the opening Carefully retain the cover and the knurled nuts 2 Slightly incline the cell holder backward to put it onto the front carrying rails of the sample compartment with the cell mount facing the detector Push the cell holder to the right hand sample compartment wall as far as it will go Throw the clamping lever 1 to the left to fasten the cell holder to the carrying rails 3 Replace the plastic foam stopper in the rear recess 3 of the sample compartm
111. ping lever Cell block with insulation Quartz window Tubes for connection to heat exchanger Cover cap Lock screws Grooves OmonN OOF WN Fig 13 6 Peltier temperature controlled cell holder with heat exchanger 13 2 4 Installation of the cell holder in the SPECORD A Lay connection cables tension free Connection cables and coolant tubes must be laid tension free Rule out tensile stress to electrical cables and bending of coolant tubes Coolant tubes and connection cables must not project into the beam paths Installing the holder in the sample compartment 1 Slightly incline the cell holder backward to put it onto the front carrying rails of the sample compartment with the cell mount facing the detector Push the cell holder to the right hand sample compartment wall as far as it will go Throw the clamping lever 3 to the left to fasten the cell holder to the carrying rails 2 Thread the coolant tubes through underneath the rear carrying rails Put the tubes into the provided ducts in the right hand sample compartment wall The tube ducts are provided with steps to achieve a higher light tightness 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 66 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell change
112. r system with cooling fins The controlling sensor used is a Pt100 measuring sensor located at the outer bottom corner of the cell block In addition to the controlling sensor the cell holder contains two further Pt100 sensors for optional monitoring of either the holder or the cell temperature The cell sensor is specially designed for standard cells with round PTFE stopper It may remain in the cell during the analytical measurement Caution Risk of distorted results When using other cells the measuring sensor may project into the sample beam thus distorting the measurement results By standard the cell holder is equipped with a magnetic stirrer which ensures fast and even temperature distribution within the cell 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 13 1 1 Safety notes The Peltier temperature controlled cell holder has been made and tested in compliance with the following standards and directives e DIN EN 61010 1 IEC 1010 1 e 73 23 EEC e 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 note
113. radually shifted and measured for instance for testing its homogeneity Here the marks on the table permit the sample to be positioned reproducibly 14 Mirror for reference measurement and protective cap 15 Point support to protect the sample surface from scratches Fig 18 2 Mirror and small tabletop 16 Quartz lens 17 Reflecting mirror 18 Plane mirror 19 Sample Strahleneingang oe doen sok s 16 Fig 18 3 Optical path in reflectance attachment front view 120 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Variable Angle Reflectance Attachment 18 3 Installation in sample compartment 1 Put the accessory onto the two rear carrying rails of the sample compartment with the clamping lever pointing frontward 2 Push it to the right hand wall of the sample compartment as far as it will go Secure it by throwing clamping lever 11 to the right 18 4 Adjusting the angle of reflection Loosen knurled screw 10 to set the sample table to the desired angular position Retighten knurled screw 10 to lock the sample table in position O Note In the angular range from 11 to 15 the beam is partly masked thus impairing the signal to noise ratio 18 5 Measuring with the reflectance attachment 1 Create the desired measurement parameter record in WinASPECT software For the reflectance measurements choose the following accessory specific options Measurement parameter Opti
114. rate the system using several certified standards same as in 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 19 5 Reflectance measurements The colored appearance or the gray tone of an opaque body is due to its wavelength dependent back reflection reflectance Reflectance measurements can be performed with different illumination and measurement geometries depending on the surface structure of the sample To preclude the effect of the surface structure as far as possible the sample surface is diffusely illuminated via the inside wall of the integrating sohere The sphere captures the radiation reflected by the sample and sends it diffusely to the detector of the SPECORD Users Manual SPECORD 200 205 210 250 Accessories 07 2005 129 Analytik Jena AG Integrating Sphere 130 The measurement geometry of 8 d d diffuse means that the surface of the sample is illuminated at an angle of 8 relative to the surface normal and the light reflected by the sample surface into the integrating sphere is diffusely sent to the detector The reflectance of the sample is the ratio of the radiation reflected from its surface and the radiation reflected from a completely matt white surface of a standard e g a Spectralon standard under the same optical conditions The integrating sphere is preferably used for ref
115. rew 4 and push support block 5 to the left stop 3 Insert sample 6 into holder so that it rests on mechanical stop 2 4 Push support block 5 towards the sample so that spring clips 3 safely hold the sample 5 Fasten knurled screw 4 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 15 Analytik Jena AG Holder for cylindrical cells 5 Holder for cylindrical cells 5 1 Description and use These holders serve for the accommodation of cylindrical cells without and with temperature control thermocell having an outside diameter of 22 mm and a length of up to 100 mm 5 2 Description 1 Support rods for cells of up to 50 mm length 2 Support rods for cells of up to 100 mm length Fig 5 1 Holders for cylindrical cells 5 3 Using the holder for cylindrical cells 1 Fill in port 2 Window 3 Connectors for thermostatting tubes Fig 5 2 10 mm thermocell cylindrical Slide the holders from to onto the mounting plate for cell holders Fig 1 1 10 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 gt see Section Thermostatted cell holder Users Manual SPECORD 200 205 210 250 Accessories 07 2005 17 Analytik Jena AG Holder for round cells 6 Holder for round cells 6 1 Description and use
116. rging of sample compartment Below a certain cell block or cell temperature dew point and depending on room temperature and relative humidity the water contained in the ambient atmosphere condenses at the cell walls and the cell block This will result in a distortion of measurement results For the beginning of condensation dew point temperature the following relation applies 9 same humidity 9 Dew point temperature in C ae a 0 1247 109 8 9p 109 8 100 9 Room temperature in C At a room temperature of 20 C and a relative humidity of 60 the dew point temperature is 12 C Condensation can be prevented by purging the sample compartment with dry gas 1 Thread a tube as thick as possible inside diameter of at least 6 mm through the front duct provided for the drain tube into the sample compartment Fig 4 1 11 p 4 1 2 Lay the tube mouth in the middle of the front sample compartment wall To prevent instable temperatures the gas must not be blown directly onto the cell changer 3 Purge the sample compartment with 800 1000 I h of dry gas e g air nitrogen or argon Note Before starting analyses at low temperatures it is advisable to pre dry the sample compartment Heat up the sample compartment by letting the Peltier temperature controlled cell changer operate for about ten minutes at 80 C Avoid opening the sample compartment unnecessarily long and thus the inflow of humid room air w
117. ribed above However the recess in the rear sample compartment wall is too small for allowing the electrical cables of two cell changers to be threaded through Therefore the accessory is supplied along with a different right angled bracket 1 Undo the right angled bracket mounted in the recess of the sample compartment In its place mount the supplied bracket Put the two supplied plastic foam strips into the recess 2 Install the second 8 cell changer in the reference beam path 3 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 85 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 86 re Connect the second 8 cell changer to the right connector in the sample compartment Both 8 cell changers use the same heat exchanger Connect the two 8 cell changers to each other by means of a short piece of tube Connect one water tube each to the heat exchanger and to every 8 cell changer Establish the connections to the heat exchanger as described above Connect the 7 pole connectors of the cell changers with the enclosed y cable Connect the plug of the y cable with the heat exchanger Connect the electrical cables to the temperature control units
118. rovided with female tube connectors 1 Connect the male connectors with the thermostatting tubes 2 Push the male connectors into the female connectors until you can hear them clicking in 3 For the connection to a fluid thermostat after insertion in the SPECORD it may be necessary to use tube adapters to compensate for any differences in tube width Disconnecting the quick lock tube couplings 4 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 34 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 6 cell changer thermostatted 10 3 3 Installation in sample compartment 3 4 5 6 2 7 1 1 Driving unit 5 Ducts for thermostatting tubes 2 Clamping lever 6 Cell holder 3 Interface cable 7 Quick lock tube couplings 4 Flat cable duct with plastic cover Fig 10 5 Installation of cell changer The description below refers to the use of a thermostatted cell changer with magnetic stirrer If you do not intend to install these components skip the corresponding item Caution Lay thermostatting tubes properly Lay the thermostatting tubes in the sample compartment so that they neither hinder the movement of the cell changer 1 Lay the thermostatting tubes underneath the front and rear carrying rails Threa
119. rs Peltier temperature controlled cell holder with heat exchanger Connect the tubes to a thermostat We recommend using quick lock couplings that allow drip free connection and disconnection of the thermostat 3 Replace the plastic foam stopper in the rear recess of the sample compartment by the plastic foam strips supplied along with the accessory 4 Thread the electrical cables 2 to the back underneath the carrying rails Put the cables between the plastic foam strips in the rear sample compartment wall 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 SPECORD with recess underneath the sample compartment cover 5 Thread the cables through underneath the sample compartment cover and put the cable into the recess so that they are not squeezed when you close the cover SPECORD without recess underneath the sample compartment cover 5 Remove the knurled screws from the cover prop Fold the cover backward Put the connecting plug of the electrical cables 2 through the slit between sample compartment cover and SPECORD basic device Screw on the cover prop again Remove the cover cap from the opening in the sample compartment cover Put the electrical cable through the slit in the opening Slip the annular stopper over the electrical cables and insert it with the slit on top into the opening Fig 13 4 p 59 6 Conne
120. s The measurement in the respective cell will be started only after you added the starting substance Activate this checkbox if you intend to record a slow kinetic reaction in cyclic measurements in all samples in a staggered mode Section Fehler Verweisquelle konnte nicht gefunden werden p Fehler Textmarke nicht definiert Cell changer moves to the first position Cell changer moves to the next position Starts the adjustment of the 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 1 Choose the measurement parameters according to your analytical needs Switch on the temperature control unit and the heat exchanger at the power Adjust the desired temperature on the temperature control unit Section Settings The measurement procedure is analogous to that with the water thermostatted 6 2 switches located at the back panels each sd on temperature control unit p 91 4 cell changer Section 5 Measurements with the 6 cell changer p 38 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 13 4 Peltier temperature controlled 8 cell changer oe SPECORDP 210 1 Temperature
121. s accommodating the reference s The selected positions appear beside the Reference button Maximum number of selectable references 10 110 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG APG 53 100 XYZ Autosampler Taking the sample measurement 1 Load the samples on the sample rack and insert the rack in the autosampler 2 Start the measurement by a click on the corresponding toolbar button on the WinASPECT desktop The measurement is started immediately The reference measurements are performed and considered according to the options selected in the measurement parameters 15 6 Finding the appropriate pump time To find the appropriate pump time use a liquid having a viscosity similar to that of the sample to be analyzed 1 Puta vessel containing the test liquid in the sample holder 2 With the sampler switched off move the guide arm of the device over the vessel and push the aspiration tube holder down as far as it will go so that the aspiration tube dips into the test liquid To ascertain the optimum pump time use the parameter options of the sipper 3 Inthe Device Driver on the Accessories tab choose the Sipper option 4 Choose the desired Pump time and save the measurement parameters 5 Start a measurement by a click on the corresponding button on the WinASPECT desktop 6 Watch whether the liquid has flown through the cell The pump time is optimum if about 2
122. s and the notes marked by symbols A 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 Earth conductor required Only connect the device to a power outlet with earth conductor to ensure operation as per Protection Class I earth conductor connection Do not make the protection ineffective by the use of extension cables without earth conductor Correct fusing Only use fuses of the specified type and rating Section Technical data of Peltier temperature controlled cell holder air cooled p 56 Warning Do not operate the equipment in explosion risk rooms Warning Risk of burns gt gt Before replacing the cell after operation at higher temperatures wait until it has sufficiently cooled down There is the risk of burns Caution Accumulation of heat gt Accumulation of heat might result in overheating and faults on the device Make sure that you do not cover the ventilation slots of the control device and of the heat exchanger of the cell holder Caution Handling liquids Take care that no liquids can get into the control device to avoid damage of the device 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 th
123. scan Activate this checkbox if you intend to record a slow kinetic reaction in cyclic measurements in all samples in a staggered mode Fehler Verweisquelle konnte nicht gefunden werden p Fehler Textmarke nicht definiert Pos 1 Cell changer moves to the first position Pos 1 Cell changer moves to the next position Adjustment Starts the adjustment of the cell changer Parking When two Peltier temperature controlled 8 cell changers have been installed they can be used in two modes In synchronous mode every sample will be analyzed against a specific reference In staggered mode the number of samples in a measurement series increases to a maximum of 14 For this in the measurement parameters on the Accessory tab the 2x 8 cell changer must be selected The possible modes are described in Section Use of two 8 cell changers p 45 13 4 6 Measurement procedure 1 Choose the measurement parameters according to your analytical needs 2 Switch on the temperature control unit and the heat exchanger at the power switches located at the back panels each 3 Adjust the desired temperature on the temperature control unit gt Section Settings on temperature control unit p 91 4 The measurement procedure is analogous to that with the water thermostatted 6 cell changer Section 5 Measurements with the 6 cell changer p 38 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 89 Analytik Je
124. sert the sohere body in the SPECORD and move it to the right as far as it will go against the cell mount in the sample compartment Fig 1 1 10 Reflectance measurement procedure 132 The measurement procedure is similar to that of transmittance measurements If you want to measure the diffuse reflectance as relative quantity in order to compare two only slightly different surfaces it will do to perform a reference measurement with a purely white Spectralon standard and subsequently take the sample measurement Insert the reflector into the round aperture in the rear mount for the cell holder as described above 1 Inthe Device Driver dialog of WinASPECT software create the desired measurement parameter record For the reflectance measurements choose the following accessory specific options Measurement Option to be activated parameter Correction Reference Slit As wide as possible to obtain a good energy level Accessory Integrating Sphere 2 Insert the two Spectralon inserts for gloss trap Fig 19 1 18 and reflectance aperture Fig 19 1 22 in the sphere body 3 Carry out a reference measurement For that you may use a standard 4 Ifyou have to analyze a powder sample fill it into the corresponding holder Fig 19 1 21 outside the SPECORD Accommodate the sphere body in the sample loading fixture Fig 19 4 Attach the holder for powder samples to the sphere body 5 Make sure to install the soher
125. sphere condenses at the cell walls and the cell block 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 87 Analytik Jena AG Peltier temperature controlled cell holders cell changers Peltier temperature controlled 8 cell changer 9 Dew point temperature in C sae humidity Vo clean 100 0 1247 109 8 9p 109 8 9 Room temperature in C At a room temperature of 20 C and a relative humidity of 60 the dew point temperature is 12 C Condensation can be prevented by purging the sample compartment with dry gas 1 Thread a tube as thick as possible inside diameter of at least 6 mm through the front duct provided for the drain tube into the sample compartment Fig 4 1 11 p 4 1 2 Lay the tube mouth in the middle of the front sample compartment wall To prevent instable temperatures the gas must not be blown directly onto the cell changer 3 Purge the sample compartment with 800 1000 I h of dry gas e g air nitrogen or argon Note Before starting analyses at low temperatures it is advisable to pre dry the sample compartment Heat up the sample compartment by letting the Peltier temperature controlled cell changer operate for about ten minutes at 80 C Avoid opening the sample compartment unnecessarily long and thus the inflow of humid
126. st take a reference measurement inserting the provided mirror in place of the sample 18 2 Design and operating principle 1 Base plate 7 Scale for reproducible sample positioning 2 Table 8 Scale for adjusting the angle of reflection 3 Large tabletop 9 Index for reading the set angle of reflection 4 Sample holding clip 10 Knurled screw for locking the angular setting 5 Marks indicating the illuminated sample 11 Clamping lever area for defined angles of reflection 12 Beam entrance 6 Measuring aperture 13 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 119 Variable Angle Reflectance Attachment The sample table can be swiveled horizontally to vary the angle of reflection in the range 11 60 The optical path of the measuring beam is the same for all angles that can be set You can slide either a large tabletop with small measuring aperture preferably for small samples or a small tabletop with large measuring aperture preferably for larger samples onto the table The samples are clamped to the tabletop The large tabletop rigidly lies on the table during the measurement The marks on the tabletop provide reproducible positioning of the sample The small tabletop permits the sample on the table to be g
127. 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 7 Thread the electrical cables 3 to the back underneath the rear carrying rails Put the cables between the two plastic foam strips in the recess in the rear sample compartment wall 4 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 SPECORD with recess underneath the sample compartment cover 8 Thread the cables through underneath the sample compartment cover and put the cable into the recess so that they are not squeezed when you close the cover SPECORD without recess underneath the sample compartment cover 8 Remove the knurled screws from the cover prop 5 Fold the cover backward Put the connecting plug of the electrical cables 3 through the slit between the sample compartment cover and the SPECORD basic device Screw on the cover prop again Remove the cover cap from the opening in the sample compartment cover 2 Put the electrical cable through the slit in the opening Slip the annular stopper over the electrical cables and insert it with the slit on top into the opening Fig 13 4 p 59 9 Connect the temperature control unit and the heat exchanger see Sections Connection and operation of temperature control unit p 90 and Connection and operation of t
128. t 5 Put the sipper into the sample compartment and connect it Inserting the sample tube Before adjusting the sample tube make sure the autosampler is switched off The sample tube is supplied ready for use The tube consists of e anMFA tube for sample transfer e the tube connection to the flow cell silicone tube with black stopper and e apiece of tube for stabilization black and improved guidance of the MFA tube 1 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 8 APG 53 100 XYZ Autosampler In the following adjustment take care that the MFA tube is not displaced within the guide tube and the above lengths be kept Slip the Tygon tube piece of the sample tube over the inlet connector of the flow cell In connecting the tube observe the directions of flow possibly marked on the flow cell Thread the MFA tube together with the tube for stabilization from inside through one of the ducts Fig 1 1 12 in the front wall of the sample compartment to the outside For the time being clamp the guide tube only loosely in the tube holder 12 of the XYZ autosampler Insert a Sample cup in the sample tray With the autosampler switched off move the guide arm 15 of the tube holder until the sample tube is in the middle above the sample cu
129. t the zeroth order of light in the optical path gt Section Adjustment of zeroth order p 8 For visual observation insert an approximately 10 mm wide strip of paper in the cell cavity for turbid samples and from top look at the beam passing through Successively turn the screws for vertical Fig 14 1 4 and horizontal adjustment Fig 14 1 12 Then carry out an energy measurement for fine adjustment 3 Activate the menu command Measurement Set Parameters to create a parameter data record with e g the following settings Wavelength 500nm Integration time 0 1s Slit 2nm Correction No Cycle automatic 5 Display Energy 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 Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Cassette sipper 14 4 Sample measurement 14 4 1 Settings on the PC In the device driver choose the following accessory specific measurement parameters 1 In WinASPECT software open the device driver 2 Choose the general measurement parameters slit wavelength ordinate display etc 3 As correction mode choose either Reference or Special correction based on a stored file 4 On the Accessory tab choose the Sipper option This will bring up the foll
130. t to measure samples in cells you can vary the height of beam transmission through the cell by adjusting the stop Fig 19 1 4 In this way you can set the following beam heights 8 5 and 15 mm For the transmittance measurement of larger solid samples you may remove the stop Fig 19 1 4 and the knurled screw on the Spectralon insert Fig 19 1 18 You can place the sample onto the thus arising smooth surface Preparing the measurement 1 First insert reflector Fig 19 1 20 as far as it will go into the round aperture in the middle of the rear mount for the cell holder The flange of the reflector should rest on the mount 2 Insert the Spectralon insert 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 3 Adjust stop Fig 19 1 4 to the desired beam transmission height 128 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG Integrating Sphere 4 If required by the type of sample unscrew the stop Fig 19 1 4 and the knurled screw on the Spectralon insert Fig 19 1 18 5 Place the integrating sphere onto the two front carrying rails and push it to the right as far as it will go Make sure to position it reproducibly against the stop for every measurement Insert the unit in the way appropriate for the type of sample to be analyzed Position for transmittance measurement of solid samples I
131. tical adjusting screw 11 5 Sample aspirating tube 12 6 Tube cassette 13 7 Pump rollers 14 Fig 14 1 Design of cassette sipper The cassette sipper consists of Eccentric Ready made pump tube with stoppers Drain tube Clamping lever Horizontal adjusting screw Cell retaining spring Connecting plug e Adjustable holder for flow cells of 1 2 and 5 cm pathlength e Peristaltic pump e Tube set User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 97 Cassette sipper 14 3 Mounting the cassette sipper 14 3 1 Mounting the tube set 98 1 Sample aspirating tube 4 Tube cassette 2 Flow cell 5 Eccentric 3 Pump tube 6 Drain tube Fig 14 2 Tube set for cassette sipper Mount the tube set as illustrated in Fig 14 2 1 2 4 Fasten the pump tube in the tube cassette by tensioning it between two stoppers Fix the sample aspirating tube to the flow cell To this end slip the Tygon tube end over the inlet connector of the cell observe the marking indicating the direction of flow on the cell The black Viton gasket must rest on the inlet connector and the Teflon tube project into the cell This is to prevent that a sample reservoir forms at the inlet connector which would cause measuring errors by carry over Fix the pump tube with the tube adapter and the short silicon tube to the outlet connector of the cell In doing so observe the proper direction of the tube cassette If the
132. tier temperature controlled B Cell CNaANGeh teeta eee le ei a i ee te 87 Options for Peltier temperature controlled 8 cell changer for SPECORD 88 Back panel of temperature Control unit cccceeeeeeeeeeeeeeeeeeeeseeeeseeeeeens 90 Front panel of temperature Control UNIt ccccseeeeecseeeeeeeeeeeseeeeeeseeeeeess 91 Temperature distribution in cell block and in cell for different types of cells measured on air cooled Peltier temperature controlled cell holder 92 Heat exchanger front Danell cccccccssseeccesseecceeeeeceeeeeeceeeeeeseeseesseneeeens 94 Heat exchanger rear panel ccccssccccceseecceeseecceesecceeeeeeceeeeesseeeeesseneeeees 94 Design Of cassette SIDPEN ccccccseececceeseeceeeeeeceeeeeeseueeecseeeeesseeesseaeeeens 97 Tube set for cassette SIDDEN hace eccs ceed eee ndecs esate ened cans eden chadeceaence ye 98 Cassette sipper mounted in SPECORD ccccccceseceseseseeseceseseststesererereees 99 Device driver Accessories tab with selected Sipper option 0 101 APG 03 TOME VIEW tase seu tances e a a AER 106 Connections of APG53 rear Panel ccccceeesesseeeceeeeesseeeeeeeeeeeseaaeneees 107 Accessories tab APG 53 SeleCted cccccccsseeeeeeeeeeeeeeessaeeeeeeeeaeeeeeeeeas 110 Fiber coupling adapter with Measuring PrOobe cccceceeeeeeeeeeeeeeeeeees 113 Absolute reflectance attachment cccccccccsseeeeeeeeeee
133. ts samples into the beam Measurement parameters for staggered operation 46 Cell changer First sample i 4 FY Pos 1 Last sample A _ Na 14 8 Fos 1 Ist sample Reference M l Synchron Manual Start T Adjustment Slow time scan Parking Fig 11 3 Software settings for the combination of two 8 cell changers in staggered operation In staggered operation the Synchronous option must always be deactivated Using the First sample and Last sample slider buttons you can set up to 14 cell positions Beside the slider bar the number of the sample and its position on the two changers is displayed R denotes the cell changer in the reference beam path and M denotes the cell changer in the sample beam path e g R1 first position of the cell changer in the reference beam path In the presentation of the currently selected measurement parameters on the WinASPECT workplace the assignment of cell positions is displayed according to your choice Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 8 cell changer Accessory 28 B cell changer First sample 1 Last sample Cell changer 1st sample Reference Fig 11 4 Measurement parameter presentation on WinASPECT workplace Beginning with the first position of the cell changer in the reference beam path load the cells continuously on the following cell positions In the measurement parameter display the following abbreviations are used f
134. ure that the electric cables are not tensioned and the coolant tubes are not folded Take care to ensure that the coolant tubes and the connecting cables do not project into the light path of the sample or reference beam path 1 o N Replace the plastic foam stopper in the recess in the rear sample compartment wall 4 by the two plastic foam strips supplied along with the accessory Turn the knurled screw 7 clockwise as far as it will go 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled 6 cell changer 4 Clamp the cell changer to the carrying rails by turning the knurled screw counterclockwise Fastening the knurled screw hand tight will do to lock the cell changer reliably 5 Thread the cable with connector to the SPECORD 5 underneath the rear carrying rails and connect it to the left connector on the sample compartment wall 6 Lay the coolant tubes underneath the rear carrying rails Thread them through the provided ducts in the right hand sample compartment wall 6 The tube ducts are provided with steps to achieve a higher light tightness If the tube is caught on these
135. ushions are forming when filling the coolant system which disappear only after several minutes Briefly switching the device on and off may accelerate the removal of these air cushions 13 6 3 Replacing fuses on the heat exchanger Replace any defective fuses on the heat exchanger by following this procedure 1 Disconnect the power cable 2 Open the fuse holder by pulling its lid 3 Replace the defective fuses considering the technical data of the cell holder or the cell changer you are using 4 Close the fuse holder again 5 Reconnect the power cable 6 Switch the SPECORD on again User s Manual SPECORD 200 205 210 250 Accessories 07 2005 95 Analytik Jena AG 14 Cassette sipper 14 1 Intended use Cassette sipper The cassette sipper rationalizes manual laboratory work in laboratories with medium sample batches Sample feed is computer controlled A peristaltic pump transfers the sample for the measurement into the flow cell After the measurement the sample is pumped into the waste bottle Sample feed can be manual or automatic by an autosampler The cassette sipper can also aspirate sample and reference simultaneously In this case equip the pump with two tube cassettes and place the reference cell in the adjustable cell holder in the reference beam of the SPECORD 14 2 Design of cassette sipper 6 10 1 Flow cell 8 2 Inlet connector of flow cell 9 3 Outlet connector of flow cell 10 4 Ver
136. uves eeeceaen kets 100 14 4 SAMPIE measurement aren E 101 14 4 1 SENOS OM MS PG anea a Saeadee isa etaenceccgats 101 14 4 2 Performing a sample measurement ccecccceeeeeceeeeecceeeeeceseeeceseesssaeees 102 14 5 are ANG MaAmMmenanGOns 2n42 Jette ddas at ered Aled dan fale a 103 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 3 Analytik Jena AG Contents 15 15 1 15 2 15 3 15 4 155 15 6 16 16 1 16 2 16 3 16 4 16 5 17 17 1 17 2 17 3 17 4 17 5 17 6 17 7 18 18 1 18 2 18 3 18 4 18 5 18 6 18 7 18 8 18 9 19 19 1 19 2 19 3 19 4 19 5 19 6 20 APG 53 100 XYZ AutoSampler ccccssseseeseeeeseeees 105 intended MSS eana T ATN 105 DAIS IY OLE E hea a a a a e a a aetaa eee 105 Design and installation of the APG 53 100 ccccceceesesseeeeeeeeeeseeeeseeeeeees 106 Connecting the XYZ autosampler to the SPECORD oo 108 Sample measule meN csar E 110 Finding the appropriate pump tiMe ssessssssssnrseesrnrrrsrrrrrrsrnrrrerrrrreerrrnreee ne 111 Fiber coupling for measuring probes ccesseeees 113 DeScripltiOn and USG 2k a E a a a 113 Design and function of fiber coupling with measuring probe 00008 113 Design and function of the fiber coupling with SMA connectors 05 114 Installation of the adapter in the sample compartment cccecceeeeeeeees 114 Alignment of fiber coupling c ccsccccsssceccesseecceeeee
137. versal holder 3 After you have attached and clamped the universal holder slide the cell holder or the solid sample holder onto its mounting plate Cr Note It is necessary to position the universal holder at the right hand wall of the sample compartment if the inserted sample shall be analyzed in the position where the beam cross section is minimal This position ensures optimum signal to noise ratio If you want to arrange the sample in a different position you can slide the universal holder to another place on the carrying rail and clamp it there 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 12 User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG 100 mm cylindrical cell absorption tube 3 100 mm cylindrical cell absorption tube 3 1 Description and use The cylindrical cell serves for measuring liquid samples requiring a pathlength of 100 mm The effective pathlength of the cell in cm is engraved to the cell body The 100mm cylindrical cell comes with a special holder 1 for cylindrical cells 3 2 Description 1 Holder for cylindrical cell 5 100mm cylindrical cell 2 Universal holder 6 Filling port with stopper 3 Clamping lever 7 Effective pathlength of the cell 4 Mounting plate of universal holder Fig 3 1 100 mm cylindrical cell 3 3 Inserting the 100mm cylindrical cell 1 Put the universal hol
138. wivel mirror Stop screw for W beam configuration O A OO N Fig 17 1 Absolute reflectance attachment User s Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG ONO Stop screw for V beam configuration Fixed mirrors Clamping lever Stop screw to sample compartment wall Sample holder 115 Absolute Reflectance Attachment 17 3 Installation in sample compartment A Caution Contamination of mirrors Do not touch any mirror surfaces 1 Put the accessory onto the front carrying rails of the sample compartment with its clamping lever 8 pointing frontward 2 Push the accessory to the right hand wall of the sample compartment as far as it will go Secure it in position by throwing over clamping lever 8 to the right 17 4 Operating principle The absolute reflectance of the sample is determined in two steps W beam configuration V beam configuration Reference measurement Sample measurement Fig 17 2 Beam geometry in Absolute Reflectance Attachment Reference measurement m Without any sample inserted turn carrier 3 with swivel mirror 4 up to the stop of the V beam configuration Sample measurement m Turn carrier 3 with swivel mirror 4 by 180 in the position for W beam configuration m Withdraw sample holder 10 from locating plate 2 Put sample 1 to locating plate and let sample holder return until it touches the sample The measurement is taken at
139. y analogy with quantitative analysis For the calibration certified standards should be used 19 4 Transmittance measurements The integrating sphere causes even illumination of the detector surface in the spectrometer independent of any influence scatter deflection of the beam through the sample In this way the accuracy of results is improved For the analysis of solid transparent samples of a large optical pathlength measurements with the integrating sphere are the only way to avoid the systematic measuring error otherwise caused by the influences on the beam Fig 19 2 illustrates the optical path in transmittance measurements of a scattering sample Users Manual SPECORD 200 205 210 250 Accessories 07 2005 127 Analytik Jena AG Integrating Sphere Fig 19 2 Optical path in transmittance measurements 1 Mirror 2 7 Reflector 2 Mirror 3 8 Detector of SPECORD 3 Cell with scattering sample 9 Baffle plate 2 4 Baffle plate 1 10 Spectralon insert for reflectance aperture 5 Spectralon insert in place of gloss trap 11 Mirror 1 6 Non scattered radiation 12 Beam path of SPECORD Baffle plate 1 Fig 19 2 4 prevents the direct light of the sample from being incident on the detector surface Baffle plate 2 Fig 19 2 9 prevents the light not scattered by the sample from being incident on the detector of the SPECORD after the first reflection by the SPECORD insert Fig 19 2 10 If you wan
140. y desired cell position Take the connector Fig 13 14 2 from the storage receptacle Fig 13 13 3 and plug the connector onto the cell measuring sensor 3 Onthe temperature control unit switch the selector switch to cell 4 Ifyou no longer need the cell sensor disconnect it from the connector and plug it into the storage receptacle Fig 13 13 3 Fault indication If the temperature displays Fig 13 17 2 and 3 on the control unit are flashing either the cell measuring sensor has not been connected properly to the connector or the sensor is defective Operation without heat exchanger When operating the Peltier temperature controlled 6 cell changer without heat exchanger or with the heat exchanger switched off cooling is electronically suppressed heating however is possible In this case if the ambient temperature is constant and the selected nominal temperature is about 5 degrees above room compartment temperature the selected nominal temperatures can be kept to an accuracy of 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 on p 81 refers to the operation of the cell changer with heat exchanger Operation with purging of sample compartment Below a certain cell block or cell temperature dew point and depending on room temperature and relative humidity the water contained in the ambient atmo
141. y means of the supplied cell sensor 2 Put the cell into the cell block and close it by means of the cover cap the grooves are facing the lock screws 3 Lock the cover cap by slightly twisting it 4 On the temperature control unit switch the holder cell temperature selector to cell Extending the immersion depth of the measuring sensor 13 1 5 Care 60 The contact cap Fig 13 2 10 is fixed in the cover cap with a grub screw By loosening this screw you can vary the immersion depth of the contact pins in the cover cap by maximally 4 mm This allows the cell sensor to be used in a certain range also for non standard cells The cell holder is largely maintenance free e Handle sample substances carefully to avoid contamination especially inside the cell block e f despite all care sample substance is spilt instantly wipe it away with absorbent cloth or paper e f despite all care the cell holder should become contaminated e g by sample substance you may clean the interior of the cell block with ethanol or water plus a dash of a detergent 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 Peltier temperature controlled cell holders cell changers Peltier temperature controlled cell holder air cooled 1 Base plate 3 Draining screw with gasket 2 Guid
142. ying operating manual provided by the manufacturer 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 105 Analytik Jena AG APG 53 100 XYZ Autosampler 15 3 Design and installation of the APG 53 100 106 14 15 13 12 11 2 10 3 9 4 Fig 15 1 XYZ autosampler basic unit Screws 4x for fastening the base covering Base covering for the accommodation of the sample rack and for covering the motion range of the magnetic stirrer bracket Knurled screws 4x for fastening the feet of the device in the foot sockets Plastic fork 2x for fastening the base covering to the feet of the device Foot of basic unit Sample tray for the accommodation of 53 sample cups and 1 rinse vessel Sample cup Aspirating tube Knurled screw for fastening the stirrer bracket to the Z dome 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 APG 53 front view Users Manual SPECORD 200 205 210 250 Accessories 07 2005 Analytik Jena AG APG 53 100 XYZ Autosampler XYZ autosampler basic unit 2 Screws 4x for fastening the base covering to the device 4 Knurled screw 4x for fastening the feet of the device in the foot sockets

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