FR559 Crystal heater user manual
Contents
1. FR559A Crystal Heater User manua 0559751 FR559 Crystal heater for use with CAD4 serial number 538 16 nn and up For installation on KappaCCD or KappaApex systems visit http www bruker axs nl select Support and download click Literature click Bruker AXS B V The Netherlands login or register and select KappaCCD technical user manual The Crystal heater consists of e Aquarium air pump capacity 3 litres min These pumps contain an electromagnet and a bellow They operate only at a specific mains frequency for which they have been designed The output of a 50 Hz pump on a 60 Hz supply and vica versa is less than 50 of the nominal flow Bruker AXS Delft supplies only pumps for 50 Hz mains supplies Users in 60 Hz mains areas have to procure such a pump from a local aquarium pet shop e Controller Check the mains voltage on the serial number label before connecting it to the local mains e Eucentric goniometer head with heater and themocouple plus a heater base for use on other goniometer heads e Phi limit switch set for use on the CADA Air supply To reduce the pulsation of the air stream from the pump put a small glass bottle not delivered volume 0 3 0 5 litre between the pump and the heater m PRESSURE CRUGE I b i le d F m HT I it i REN NG i Kl 4 e Bal N ar A CASTEL fi o fo HERTER A ob s DS me P a i BOTTLE The pressure should be in the2. 2277 gt SSS SEM he K 4 2 a r s psd A A 4 a IN IN ER l AE l EEE f r E J H Dr HE rea tai ed SR FEO EERE nam ga f Lf Pe JEr a Esta a4 a a P LAME T om pl MZ VE l 6 ALS SAY E AV Llor i 63 96 Y __ Y a MOT tg Le EEE EEE To re build the eucentric nm em goniometer head for regular nen em use see the drawing on the left The encircled parts are packed with the spare heater elements earls 500 Boon PHI BH Cho EHH Gc Sample position approx 4 mm above the nozzle Overall height 1516 918 goniometer head with heater 63 96 mm compatible with CAD4 MACHS KappaApex goniometers For instruments with 49 mm eucentric height use low XYZ goniometer heads Mounting the limit switch unit Remove the Phi coarse scale disk at the back of the Kappa block There is one screw in the centre of the block and one lateral screw Remove the dripping tray at the base of the kappa support block if present Position phi to O degrees Mount the switch unit using the support bracket and 2 screws see picture TPE EN YE LT IA ZARA RS y SISNS m SES Now the disks supplied must be mounted on the phi axis the largest one first phi should be at 0 degrees during this operation There is a cam in the smallest disk that fits a slit in the largest disk A Ther
3. at position to phi 270 With the new set up phi should go to 270 via O e When not OK restart the CAD4 program a second time before starting to correct the hardware installation Glue The sample is fixed on a quartz fibre and the fibre is attached to a metal pin e Sample to fibre bond Cerastil C 3 1100 C or C 10 1650 C www panacol de or a 50 50 mix of waterglass and manganese oxide 800 C can be used to fix the sample to the quartz fibre e Fibre to metal pin bond Torr Seal Resin Sealant Varian part number 9530001 can be used for the quartz metal bond www varianinc com temperature range 45 C to 120 C Temperature calibration See the original publication by F Tuinstra and G M Fraase Storm J Appl Cryst 1978 11 257 259 some older literature about HT experiments mentions mounting crystals of known melting range and observing the start of the melting with the aid of a microscope Crystals used were Diphenylacetylene m p 61 62 C Urea 132 5 134 5 C Thiourea 171 171 8 C AgNO3 212 C NaNO gt 2 1 C NaNOs 307 C KNO 440 C NaCN 562 C Nal 650 C
4. e is a Allen screw at the side of the smallest disk that can be loosened during mounting B It is important to position both disks correctly the cam on the small disk should be close to the small vane C that is visible under the switch unit The vane has 2 micro switches that sense the left and right movement of the vane see scheme phi limit switch Because of the cam and slit this implies the protruding part of the biggest disk will be at the opposite side Once both disks are in position and fixed to the phi axis the Allen screw can be tightened B In the CAD4 program go to CASPAR and set phi limit switch present The top angle of the goniometer head with the heating device is 90 and the maximum radius to 30 mm Do not use larger goniometer heads to prevent crashes outside the regular collision collars Fix the connector of the switch unit to the socket marked Limit switch at the back of the goniometer During standard use a dummy plug is in this socket it must be put back after removing the limit switch unit C 4 POS SWITCH OPEN 21 yp NEG SWITCH CLOSED Phi limit switch diagram e Enough slack should be kept for the several cables running between the limit switch unit the heater and the outside world also when moving omega and kappa e Restart the CAD4 program Check the proper operation of the limit switch without the heater The phi range is now limited to 240 lt phi lt 240 Position phi 180 and from th
5. order of 50 100 cm water column Controller All controls are located on the front of the controller The LCD screen displays e The selected temperature for the experiment switch in position SET POINT e The actual temperature switch in position MEASURED e The current through the heating element press button HEATER CURRENT The green LED SET POINT lights up at the selected temperature The knob ADJUST sets the temperature for the experiment on display when switch in position SET POINT The red LED ALARM lights up when the thermocouple is disconnected or when the actual temperature and the set temperature differ too much for a too long period The push button RESET clears the electronics after the cause of the alarm has been corrected E g loose electrical connections no air broken heater element The black and red connectors are the outputs to the heater element The connector TC is the input from the thermocouple The recorder output is 1 V 100 C For more information about the controller consult the service manual 0559750 Goniometer head with heater A special connection piece ensures a stable mounting on the eucentric goniometer head 1516918 left It screws on the goniometer head after removal of the upper height adjustment locking ring and pin The universal heater support right can be used with goniometer heads from other vendors E ay PZZ227
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