kyroflex2 - X-ray Diffraction Texas A & M University
Contents
1. Tuning The Temperature vs Time graph shrinks slightly and the Zoom Fine Tuning tools show up in the new space created Figure 10 K KRYO FLEX Control Running E 21x File BIS Advance d Options r Liquid Nitrogen Dewar r Temperature vs Time Temperature N2 Flow gt 300 250 2 amp 200 o Qa 5 150 100 08 50 00 08 55 00 09 00 00 09 05 00 09 10 00 Automatic Time HH MM SS 1505 Dewar Refill Force Refill To Start Zoom of temperature scale in degrees i a Zoom Temperature Scale 100 Z p 2 Temperature Units Set Temperature ce a Show all temperatures in ne Target Temperature 100 Curent Temp Rate Status Koo Bs _ Figure 10 Zoom Fine Tuning tools appear under graph 2 Check or uncheck the Zoom Temperature Scale box of the new tools to turn on or off the zoom When the Zoom Temperature Scale box is checked the Temperature vs Time graph will be zoomed in on the target temperature according to the scale settings 3 Enter a scale value in the Zoom of temperature scale in degrees field Figure 11 or adjust the slider bar below the heading Zoom Temperature Scale ons m Temperature vs Time 100 1 100 0 8 08 50 00 03 00 00 03 10 00 09 20 00 03 30 00 Time HH MM 55 Temperature K oo to co The temperature scale is zoomed in Zoom of temperature scale in degrees K g M Zoom Temperatur2. forms see Figure 1 example near 300 mark to mark the exact temperatures at different points along the timeline Two light lines form see Figure 1 example near 100 mark lines are so close they appear as one to indicate the acceptable range of temperatures for the current target temperature the range being target temperature 0 1 These lines appear on the graph so that you can visually verify the temperature stability During non cooling temperatures will rise to room temperature and these will record in the graph for the extent of that period Automatic and manual zoom modes allow you to view the graph to monitor operation or check particular information The graph automatically zooms out displaying the entire range of temperatures cooling and non cooling when the temperature is not stable and zooms in displaying the temperature range acceptable for stable operation when the temperature has stabilized at the target temperature This auto zoom feature allows you to readily see the current temperature in relation to previous temperatures for stability monitoring that is to see the temperature s likely rate of change You may also manually Zoom in on or out of the graph and see temperatures over a period of your choosing To zoom in on a specific period left click drag across the temperature points you wish to magnify Upon releasing the mouse your selected area will enlarge and fill the subwindow This fea
3. BRUKER ADVANCED X RAY SOLUTIONS KRYO FLEX Low Temperature Device for D8 PLATFORM User s Manual Purpose These instructions cover use of the KRYO FLEX Low Temperature Device software which controls the low temperature device and dewar that cool the sample for various applications NOTE This procedure assumes that the KRYO FLEX software which may be a standalone program or part of the PROTEUM program suite has been installed on your system Responsibilities All procedures are to be performed by general users site administrators and trained Bruker AXS personnel Disclaimer All configurations and specifications are subject to change without notice Referenced Literature e none KRYO FLEX Control Running Fie BIS Advanced Options Liquid Nitragen Dewar Temperature vs Time 300 Temperature K hm i co am CS eS T mm 100 Automatic Dewar Refill Force Refill To Start Temperature Units 9 ss snow all temperatures In Figure 1 KRYO FLEX Control Running window M86 E01034 0302 08 46 00 O8 400 08 48 00 08 49 00 08 50 00 08 51 00 08 5200 08 53 00 Time HH MM S 5 Set Temperature Target Temperature Current Temp 1 Features Before using the program you will want to be familiar with the main window Figure 1 and its features This section explains those features Temperature Units The Temperature Units subwindow allows you to select t
4. Y TEL 1 608 276 3000 FAX 1 608 276 3006 Email info bruker axs com http www bruker axs com BRUKER AXS GMBH e D 76181 KARLSRUHE e GERMANY TEL 49 721 595 2888 FAX 49 721 595 4587 E mail info bruker axs de http www bruker axs de BRUKER NONIUS B V e OOSTSINGEL 209 PO BOX 811 2600 AV DELFT e THE NETHERLANDS TEL 31 15 215 24 00 FAX 31 15 215 25 00 E mail info bruker nonius com e http www bruker nonius com 2002 Bruker AXS Inc All rights reserved Note All configurations and specifications are subject to change without notice M86 E01034 0302
5. e Seale Set Temperature Figure 11 Zoom of temperature scale in degrees To deactivate the Zoom Fine Tuning tools click Advanced Options gt Zoom Fine Tuning again to uncheck it 3 6 Set Temperature Offset The KRYO FLEX control assumes that the temperature of the nitrogen stream dispensed and monitored slightly above the sample is the temperature of the crystal This assumption may or may not be accurate Sometimes the nitrogen stream can warm up between the nozzle and the crystal if the nozzle is far away from the crystal If you know how much the nitrogen stream warms by taking an infrared reading at the crystal and calculating the difference between it and the target temperature you can enter this value to set the temperature offset as follows 1 Click the Advanced Options gt Temperature Offset Setting The Temperature Offset input panel appears Figure 12 EEE e R Figure 12 Temperature Offset panel 2 Check the Use an offset of box to tell KRYO FLEX to start using an offset value 3 Enter the offset value difference between infrared reading and target temperature in the field to the right of the box 4 Close the panel x and KRYO FLEX will begin using the offset 3 7 Temperature Ramping Normally KRYO FLEX cools down rapidly and may overshoot your target temperature This rapid change is suitable for most applications but could damage a crystal If your application require
6. et Temperature field as you normally would 3 Click on the Not Ramping button to enter settings and start ramping Click it later to stop ramping The Ramping Settings input panel appears Figure 14 M86 E01034 0302 2 x Ramping Settings a me Scale 10 Final Temp 100 A Figure 14 Ramping Settings panel 4 Enter in the Scale field the amount by which you will want the temperature to incrementally fall 5 Enter an end temperature value in the Final Temp field 6 Click the Use these settings and start ramping button to activate the KRYO FLEX control to use your settings The Ramping Settings panel will close and the KRYO FLEX control will start ramping 3 8 Wipe All Data From Graph The Temperature vs Time graph normally holds all data since the software was started If you run the software for prolonged periods the graph can consume a large amount of system memory which may make the software behave abnormally To free this memory you may want to periodically clear data from the graph To clear data from the graph click Advanced Options gt Wipe All Data From Graph The data will then be cleared M86 E01034 0302 ANSI RAB OMS ISO 9001 APPROVAL A A a rm o rm o Conditions for use of this mark are controlled by AOQC Moody International Inc USA BRUKER AXS INC 5465 EAST CHERYL PARKWAY MADISON WI 53711 5373 e USA TEL 1 800 234 XRA
7. he temperature units that you wish to use Two unit options are available Kelvins K and Celcius C When setting the units click on the circle next to your desired option K or C 100 Note that the change will immediately affect all temperatures in the main window Current Temperature The current temperature of the sample displays both as a thermometer that indicates the maximum and minimum range of the temperature and as text below the thermometer with the temperature displaying in those units you have chosen A flashing thermometer indicates an error related to temperature A message in the text subwindow by the Status lamps may explain the error Set Temperature The Set Temperature subwindow is where you set a target temperature which is the temperature you will want the system to cool to stabilize at and maintain throughout the experiment once you start KRYO FLEX Here you simply enter a target temperature in the provided field or scroll to a desired temperature using the arrows beside the field A range of 90 to 300 K or 183 5 to 26 5 C is allowed by the system You will be warned if you enter values outside this range or if you accidentally enter a nonnumeric value Temperature vs Time The current temperature also gets recorded in the Temperature vs Time graph center subwindow to show you what KRYO FLEX is doing over a period of time During the cooling operation a dark line
8. l temperatures in the main window 2 Set or change the target temperature by entering a new value in the Target Temperature field of the Set Temperature subwindow 3 Press the Start KRYO FLEX button to start cooling NOTE Press the Stop KRYO FLEX button when you want to stop cooling 3 2 Create a Log File 1 Click File gt Log File Settings to have the KRYO FLEX control create a log file of the recorded temperatures Figure 3 H KRYO FLEX Control Running File BIS Advanced Options Help F1 About Kryoflex Ctrl k emperature vs Time 300 Log File Settings Ctrl L ctrl E id mn oS 200 Temperature K i om oC 100 Figure 3 KRYO FLEX Control Running window The Log File Settings input panel appears Figure 4 EjLog File Settings default_log tst Open Log File Figure 4 Log File Settings panel Log File Active Clear Log File 2 Click on the browse button to select a logfile A standard Windows browse window appears to let you open a previous logfile or create a new one Figure 5 CE I y y 2x Look in fea KRYO FLEX Control te c EJ ez File name flog file txt v My Network P Files of type Text Files X Cancel Figure 5 Browse window 3 Highlight a current logfile or enter a new name in the File name field Then click Open The Log File Settings panel now shows your selected or new filename Figu
9. n which BIS is running because BIS controls the frame collecting hardware and the KRYO FLEX control runs the KRYO FLEX low temperature device The KRYO FLEX control assumes this arrangement and by default sets the host to an IP address that is universally accepted as a local connection You may however enter any network name or IP Address that you wish M86 E01034 0302 se BIS Socket Connection E x Host 127 0 0 1 oe 4 O04 Connect to BIS Figure 7 BIS Socket Connection window 2 At the Host field accept the default IP address enter the IP address for the Bruker Instrument Service or enter the host name you desire If you need to set the KRYO FLEX control back to the default IP Address click the Set To Local button 3 Click the Connect to BIS button If you have entered a valid host name the KRYO FLEX control will connect to BIS and you can close the BIS Socket Connection window To show that the KRYO FLEX control is connected to BIS the BIS lamp in the lower left corner of the KRYO FLEX Control Running window turns green 3 4 Obtain Information from System Monitor While the main window displays commonly needed information the control stores more information in the system monitor should you need to access those details 1 Click on Advanced Options gt System Monitor Figure 8 2k KRYO FLEX Control Running 21 xi File BIS Advanced Options gt Liq
10. nsor if a refill tank with sufficient liquid nitrogen is connected to the dewar To enable the refill feature simply check the Auto Dewar Refill box in the Liquid Nitrogen Dewar subwindow When the automatic refill option is enabled you can also force the refill to start and stop by pressing the Force Refill to Start button M86 E01034 0302 button text changes between Start and Stop when toggled Start Stop KRYO FLEX You press the Start KRYO FLEX button bottom right corner of the main window when you are ready to cool a sample Button text changes to Stop KRYO FLEX When you are done collecting data for a sample and no longer need to cool it press the Stop KRYO FLEX button to stop flow of liquid nitrogen Button text will change back to Start KRYO FLEX 2 Startup With the KRYO FLEX system set up as explained in the KRYO FLEX Installation Manual you should be able to run the KRYO FLEX control software to control the hardware instead of having to manually control the hardware 1 Double click the KRYO FLEX icon snowflake in standalone program thermometer in the PROTEUM program to start the KRYO FLEX program The KRYO FLEX Control Running window appears recall Figure 1 3 Operation 3 1 Basic Use To prepare the system for basic use 1 Inthe Temperature Units subwindow select the temperature unit K Kelvin or C Celsius that you wish the KRYO FLEX control to use Note that the change will affect al
11. re 6 2 xX EAYO FLES Controlslog_hi Iv Log File Active zjLog File Settings C Program Files Brukents5 i Open Log File Clear Log File Figure 6 Log File Settings input panel 4 Check the Log File Active box to tell the KRYO FLEX control to activate the log file and record the temperatures into the log file 5 Click File gt Close or the x box to close the panel and return to the Control window If at some point you wish to view or edit the logfile simply return to this panel and press the Open Logfile button The notepad appears and displays your logfile Or if you find that you are finished with the logfile at some point return to this window and press the Clear Log File button to delete the file 3 3 Connect to BIS Connected to the Bruker Instrument Service BIS the KRYO FLEX control can communicate the current temperature to BIS and other programs such as PROTEUM that also communicate with the Bruker Instrument Service This connection lets the programs record the temperature to which a crystal was cooled each time a frame from that crystal is collected To connect to BIS 1 Click on BIS gt Connect to BIS The BIS Socket Connection window appears Figure 7 to request a host name A host name is the network name or the IP address of the computer to which the Bruker Instrument Service is connected Usually the KRYO FLEX control will be run on the same computer o
12. s M86 E01034 0302 The BIS lamp shows if the KRYO FLEX control is connected to the Bruker Instrument Service If the lamp lights green the control is connected If the lamp is not lit the control is not connected Liquid Nitrogen Dewar The Liquid Nitrogen Dewar subwindow shows you the level of liquid nitrogen in the dewar and provides two options for refilling the dewar A dewar graphic shows three states at which the nitrogen supply may exist in the dewar full within operational range and empty These states are controlled by two level sensors in the dewar which detect the amount of liquid nitrogen in the dewar The first full level sensor senses when the dewar is full The second low level sensor senses when the dewar is almost empty Figure 2 shows the different stages Full Within Range Empty Full dewar Partially Empty dewar indicated by depleted indicated by fully green dewar white graphic graphic indicated by with low level partially green in red to stress graphic refill urgency Figure 2 Stages of liquid nitrogen level in dewar A flashing dewar indicates an error related to liquid nitrogen A message in the text subwindow by the Status lamps may explain the error To ensure smooth operation and prevent damage to your sample in the event that the liquid nitrogen would run out you can have the KRYO FLEX system automatically refill the dewar when the liquid nitrogen level reaches the low level se
13. s a more controlled temperature reduction you may want to use temperature ramping This feature works with a start temperature a scale temperature amount by which to slowly reduce and an end temperature When this feature is set the KRYO FLEX control will cool down to the start temperature and stabilize Then it will cool down in incremental stages by the scale that you set briefly stabilizing at each stage until it finally reaches the end temperature that you set Thus if you set a start temperature of 200 K a scale of 10 K and an end temperature of 100 K the control will cool to 200 K then cool down 10 K at a time in stages until it reaches 100 K To set temperature ramping 1 Click Advanced Options gt Temperature Ramping to activate the temperature ramping Temperature ramping controls will appear in the Set Temperature field Figure 13 E 2x File BIS A tions Liquid Nitrogen Dewar Temperature vs Time m Temperature N2 Flow Automatic 1 oo 4 P Dewar Refi 09 47 45 0947 47 0947 49 0947 51 09 47 53 09 47 55 150 Time HH MM SS Force Refill To Start Temperature Units Set Temperature 9 Target Temperature Show all temperatures in a 7 f Wes F Current Temp NotRamping Scale 10 Final Temp 173 5K 2979K orf J Start BIS KRYO FLEX Figure 13 Temperature ramping controls 2 Enter a start temperature in the Targ
14. ture is recursive meaning that you can select a time range within a time range further zoom to narrow the specific range shown When you want to return to the entire time range recorded in the chart right click N2 Flow The N2 nitrogen flow status displays as a scale in the N2 Flow subwindow and as text below the indicator The KRYO FLEX control is default set with a nitrogen flow rate of 5 liters per minute However when first cooling the KRYO FLEX control may switch to a Turbo Mode that uses a higher flow rate of 7 5 liters per minute to speed the cooling process Status Lamps In the Status subwindow two status lamps indicate KRYO FLEX operation The KF lamp indicates specific KRYO FLEX control status as follows e A lamp not lit indicates that the control is not actively cooling e A yellow lamp indicates that the control is cooling but the temperature has not stabilized A message appears next to the lamp that explains the status and states the target temperature e A green lamp indicates that the control has stabilized at the target temperature A message appears next to the lamp that explains the status Stabilization occurs when 90 of the observed temperatures fall within the acceptable range 0 1 over a period of 3 minutes e A red lamp indicates that a serious error has occurred and that the control is no longer cooling due to that error A message appears next to the lamp that explains the statu
15. uid Nitr System Monitor Zoom Fine Tuning Ctrl Z Temperature Offset Settings Ctrl O Temperature Ramping Ctrl R Wipe All Data From Graph Ctri wW Temperature r N2 Flow y F 5 Automatic Dewar Refill Force Refill To Start Temperature Units r Set Temperature 08 46 00 08 47 00 08 48 00 08 43 00 08 50 00 150 Time HH MM SS oy Show all temperatures in a Target Temperature 100 pid a Status Bis KRYO FLEX Figure 8 Advanced Options menu The System Monitor window appears giving you specific details for both the Evaporator and the Nozzle heaters It also gives you information on the dewar the nitrogen flow and the date and time Figure 9 M86 E01034 0302 Evaporator Actual emp 297 1 ActualPower 10 3 F 180 180 D 30 Nozzle Actual emp 297 02 ActualPower 57 5 P Sol a0 D 15 Target emp 100 Target emp 90 MasPower 0 MaxPower j Dewar LN Flow Autofill True Rate 0 Level stR ate Off 11 29 2001 9 50 57 AM Figure 9 System Monitor window 3 5 Use of Zoom Fine Tuning There are times when you may wish for finer control of the scale of zoom that the KRYO FLEX control uses when the temperature has stabilized Conversely you may wish to zoom in even when the temperature is not stabilized or you may wish to zoom out when it is stabilized Do so as follows 1 Click on Advanced Options gt Zoom Fine
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