(SAXS/WAXS) User Manual - Australian Synchrotron
Contents
1. 1 0 adag 0 360599 OSunJan 18 23 19 49 2009 UDEF1_2PV1 2345 1 0 0000 10000 13 900 39 700 27 951 4 8958 a D 270684 0 Pr 334039 0 Gun Jan 18 23 19 54 2009 UDEF1 2 bi 2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 with deta ils of 1 0 269952 0 0 QIE 0 SunJan 18 23 20 00 2004 UDEF1 2 P12 345 1 5002 0 0000 13 900 39 700 27 951 4 8958 10 261835 0 37 0 PA 0 Sun Jan 18 23 20 09 2099 UDEF1_2 P 1_2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 1 0 296597 0 36 0 0 Sun Jan 18 23 20 16 009 UDEF1 2 P 1_2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 ithe fi ena mes 1 0 283533 0 36 0 Asun Jan 18 23 20 23 2009 UDEF1_2 PV1 2345 1 5002 0 0000 13900 39700 27 951 4 8958 d i ao Bee Hee REM tae ome ioe ise No Za dene 1 ndan 1 20 1 13 39 27 A exposure times 10 285111 0 36 0 nJan 18 23 3 UDEFI_2 PV12345 1 5002 0 0000 13900 39 700 27 951 4 8958 1 0 2835293 0 36 0 D un Jan 18 2340 47 2009 UDEF1 2 P 1_2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 I t 1 0 0 a p Vun Jan 18 2 20 UDEF1_2 P12 345 1 5002 0 0000 13 900 39 700 27 951 4 8958 CUC 1 0 0 36 0 345424 J Sun Jan 1923 20 55 2009 UDEFI_2 P 1_2345 1 5002 0 0000 13900 39 700 27 951 4 8958 1 0 0 0 0 Sun Jan 1 23 22 38 2009 UDEF1_2 P 1_2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 ee ee ees EECH BS te 3 g 347 0 SunJAn 18 23 24 18 2009 UDEF1_2 PV1 2345 1 5002 0 0000 13 900 39 700 27 951 4 8958 BS te2. the User Office General glassware glass and plastic sample preparation containers Kimwipes and Parafilm is available in the chemistry laboratory Common solvents acids and some additional chemicals are also available however users are expected to provide the chemicals required for their experiment For specific requirements advice or a detailed list of the glassware and or chemicals available please contact local support staff Laboratory Equipment A range of equipment iS provided in the chemistry laboratory for sample preparation and storage A fumehood hotplate stirrers ultrasonic baths four decimal place balances are all available for routine sample preparation Some gases are available however users should contact support staff for any specific gas requirements prior to their experiment i Fridges an oven a hydraulic press and a diamond saw are also provided for storage and preparation manuals for all equipment are also available Additionally a Leica DME microscope is available in the chemistry laboratory for all users at the synchrotron i E er SSeS SSS e EE Ee E Ee a Ga e E SS SS SS eS eg Sample Environments Solid samples and liquids in capillaries brought by users may be readily mounted on the beamline Sample mounting is flexible and users are advised to consider their requirements prior to their experiment Samples are mounted
3. SAXS Parameters File e Inthe top menu go to File e Click on Get SAXS Parameters e Find your Parameters File C Data Your Directory sax e Open a previous data image by selecting the File menu and then Process single image e If the image loads the Parameters file is OK If not restart SAXS15 and load a Parameters file from a higher directory e Input the sample filename You should now be ready to collect data with SAXS15 ear I Vian ua as Version 1 2 05 05 2009 6 2 DATA COLLECTION EE ay eet Dt me etre et Ge fet EE ee ee Detector amp Beamstop Alignment Positioning and alignment of the detector and beam stop will be performed by the local beamline staff during the initial setup of an experiment A mask to exclude the region covered by the beamstop may be made in the SAXS15 software and masks may also be made to restrict the data to a specific region of interest Instructions for these masks may be found in the SAXS15 manual and local staff will also be able to assist in their use ransmission Scan This procedure will move the SAXS table to the correct height and take a transmission scan for the time selected i o Select Transmission using the check boxes i J e Select the desired scan length from the Expose drop down menu e Click on the Start Action button Data Collection Single Exposure This procedure will move the SAXS table to the c
4. in the specified direction The Central must be selected to gain command of button returns the camera to a Home position Single ithe camera movement and zoom i Clicking in the camera view also moves the camera i ogle Si Go Dn SONY Network Camera SNC RZ30P Ted onia Capture Trigger Setting Frame rate 2009 01 07 Wed10 29 30 Camera View View size HS 20 frames sec received 691911 ech r SE Zoom Controls Both the Wide and Tele buttons and the Slider Bar control the camera Zoom Additionally a box may be drawn in the camera view to zoom on a region of interest 3 a ee a ee ee ee eet Geen Eegeregie Get Geet l l l Camera Control The view and zoom of the camera may be controlled using the online interface The view may be adjusted using the arrows at the left of the display while the zoom may be controlled using the buttons or by Page 15 Version 1 2 05 05 2009 6 0 SAXS15 amp DATA COLLECTION Data collection on the SAXS WAXS beamline is performed using a modified version of the SAXS15 software developed at ChemMat CARS This software allows straightforward calibration definition of a region of interest or exclusion and data collection as a single scan raster pattern or following a time sequence An example interface is shown below Exposure drop down menu Used to select the desired scan eer eege duration or select Auto for an automated scan sequenc
5. will dump Only use this button in an actual electrical or radiation emergency oO m Search Point If this button is flashing it is ready to be pressed If you need to secure an area and the light is not flashing check that the double doors are closed Also check if the labyrinth keys are in the key interlock and turned to the lock position Inside hutch Ur mmm mmm mm mmm mmm rm mm mm mm mm mm mm mm mm rm rm mm mm rm mm rm mm E ees Siren When the search button is pressed the siren sounds until the search secure process is finished or aborted i Unlock Press this button to unlock the door to enter the hutch Once the hutch is unlocked the search and secure procedure must Sie followed to re lock it Strack Lamp Legend A quick straightforward reference to what the different stack lamp signals mean Search Point If this button is flashing it is ready to be pressed If you need to secure an area and the light is not flashing chec that the doors are closed and interior search point buttons hav been pressed Outside hutch D N Version 1 2 05 05 2009 PSS Control Panel All PSS functions i e shutter control search status and door unlocking are displayed and may be accessed from here The PSS Control Labyrinth Provides a safe path for cabling into the experimental hutch Users may feed their own cables into the end station through the l
6. Australian Synchrotron Small Wide Angle X ray Scattering Beamline SAXS WAXS User Manual Version 1 2 05 05 2009 LA MM kA WM kA kA kA AA AA UI UI Un UI WN h CG 6 0 On N ba d 8 0 d SAXS WAXS User Manual TABLE OF CONTENTS PERSONNEL SAFETY SYSTEM PSS PSS SEARCH amp SECURE PROCEDURE BEFORE YOUR EXPERIMENT CEHMICALS amp CHEMICAL SAFETY USER RESOURCES SUPPLIED BEAMLINE OPERATIONS CAMERA LENGTH ENERGY amp Q RANGE SAMPLE MOUTNING SAMPLE ALIGNMENT FLEA CAMERAS FLEA VIEWER SAMPLE ALIGNMENT VIA FLEA VIEWER SONY NETWORK CAMERA SAXS15 amp DATA COLLECTION STARTING SAXS15 DATA COLLECTION AFTER INJECTION INTO STORAGE RING TROUBLESHOOTING AUSTRALIAN SYNCHROTRON MAP 10 0 PHONE CONTACT SHEET Version 1 2 05 05 2009 21 23 24 1 0 PERSONNEL SAFETY SYSTEM PSS Siren When the search button is pressed the siren sounds until the search secure process is finished or aborted There are three different sirens one for a search in progress another indicating the search is completed and a third to indicate that the search is aborted or has timed out 45 seconds i Strobe Flashes when siren is sounding Alerts all personnel that ithe search procedure is in progress and to leave the hutch mergency Stop Button This button is for emergencies only as ower will be cut to the beamline and the storage ring
7. Motor Control the Flea pes Viewer may be used to move the sample stage l coo selected Once calibrated Shift Left Click moves the sample JH ON N f until the Red Crosshair is centered at the selected point eet To Calibrate Click on the Calibrate button and follow the on screen commands This involves marking a Fiducial with the Green crosshair moving to place the Fiducial in the opposite corner and marking the Fiducial again lea View Motor Control will only work when the Motor Control panel has been selected A om i Background Subtraction The Flea Viewer may perform background subtraction to highlight changes in the image for example the beam position In Image Control the Set Background button begins background subtraction with the current image used as the background The Clear Background button is used to stop background subtraction Version 1 2 05 05 2009 9 2 SAMPLE ALIGNMENT VIA FLEA VIEWER Samples on the SAXS WAXS beamline are typically aligned via camera display using the Flea View interface Such alignment is very precise and 50 micron Samples may be reliably aligned using the flea camera procedure e The Flea Viewer is used to directly image the beam position by observing fluorescence from a YAG crystal e The Red Beam Cursor is then placed to mark the centre of the l 541 l a i y JW Auto bea D I Shut
8. S exposure causes the attenuators to all drop back in repeat all of the above If a second round fails ring the on call i beamline staff member Cryocooler Alarm EPS Fault Motors not responding Ir the Cryocooler alarm sound you are made aware of an EPS fault or Motors on the beamline do not respond e g Sample Height not moving Version 1 2 05 05 2009 8 0 AUSTRALIAN SYNCHROTRON MAP Reception Es First Aid Sr LLM ki ell LL WS gt NI A i7 ae E Es WW oy 4 a h 4 SSS E j q gt bag A Fe Aen Set AA 8 d e ZE Iech SE Ge Biochemistry Laboratory Chemistry Ad Laboratory TA a Ss VW o D MAR SAXS Beamline Version 1 2 05 05 2009 9 0 PHONE CONTACT SHEET In an Emergency contact the Control Room Extension 123 First Aid Contact control room or security Extension 123 or 120 Extension Phone Number Control Room 123 8540 4123 Security 120 8540 4120 Reception 100 8540 4100 User Office 193 8540 4193 SAXS Beamline 166 8540 4166 Extension Phone Number Mobile Nigel Kirby 169 8540 4169 0488 304 427 Stephen Mudie 243 8540 4243 0488 327 066 Adrian Hawley 133 8540 4133 0427 840 661 Phone Number Alternate Rusden House 1800 217 778 9543 3511 Page 24 Version 1 2 05 05 2009
9. _ Accept Status DCM Tracking Inactive Active Energy 9 0000 kou the Stop actual numbers should agree once the Gap is set i Version 1 2 05 05 2009 8 0 TROUBLESHOOTING This section lists some common problems and suggested solutions for the SAXS WAXS beamline Try the suggested solutions in the order that they are listed If you are unable to resolve the problem contact local support staff e Ensure that the Mono Shutter is Open on the PSS control panel e Check that the Front End Shutter is open on the PSS control panel If it is i not you may need to call the Control Room to gain control of the shutter e Check the Storage Ring Current using the online facility status monitor e If unresolved contact local support staff Ensure that criteria shutter opening at the PSS control panel are met e Hutch mush be searched amp secured e Front End shutter requires authorization from the Control Room There must be no EPS errors warnings This may be checked by looking at the computer cabinets on the roof of the hutch All lights must be green e If unresolved contact local support staff e Ensure that hutch doors are closed in the correct order Make sure that the double swing doors closed and sliding doors are open at the start of 1 the search procedure ie Ensure that the labyrinths are closed and locked and that the keys are in 3 the PSS panel inside the hutch i e If unr
10. abyrinth Keys are required to unlock the labyrinth and must be replaced in order to secure the hutch Ask user Support staff for more Version 1 2 05 05 2009 1 1 PSS SEARCH amp SECURE PROCEDURE 1 Enter the end station hutch and check that no one is present 2 Ensure that the swing doors are closed and the sliding door is open 2 Press the flashing search button by the sample table The alarm will 3 sound and you now have 45 seconds to complete the search and secure A Press the now flashing search button opposite the sliding doors 5 Exit hutch and close the Sliding doors You will hear the doors lock The outside secure button will now start flashing 6 Press the secure button outside the end station hutch The indicator will now show orange and the end station hutch is secure and the siren sound will change If you accidentally unlock the front end optics hutch you will lose beam Please contact user support staff DO NOT enter the front end hutch PSS Control Panel Overview Front End Shutter Control Blue Searched Red Not Searched zouge bing HUTCH Aer HUTCH B Enabled Disabled Searched Searched Red open i BEE Beamline FE Shutters MOTTO gt DLLSeTsS Green closed Red Locked l Enabled Upened Opened oe Green Unlocked Disabled i SE q Closed Closed u Shutter control CLOSE CLOSE Dress to activate l Door locked Door locked Press to Unloc
11. e Acquire Menu I Ge 15 1 gt 54X5 WAXS 3 296 i U sed to ed it the Tools Data Detector Options Auto scan i l 5 CurfntReadIn Blank 1 2 C3 GA C5 CE CF CB CY C10 Data Directory C data l KEN Str a nd l Normalization Log File test log Param File BS_test_parms sax furent Plotted M Blank M1 M2 M3 M4 75 6 7 F 8 Fg F 10 I I l l start a M ove i Current Image Frame BS_test_2_044 tif Time Stamp SunJan18_23 24 28 Blank Subtractos I Blank IT ToT aT STET fis 3 oa l l and Scan e 1 i e Next Frame to Acq Example_A_O01 tif ax Index 44 xpose SEC e Hold a Feces Paks GR SS l i al et 5 SER o e se q uence i Next filename Example A DO H Cycle a N E E Lin lt gt Log X Axis Y Axis 4 tn x b p pm pm pm pm pm rm rm rem rm pm pm em pm pm re Filename Must end in Zog eg the 001 tif ending denotes ithe first scan of anew sample a x ch CH gt Radially averaged D Image from detector data profile an a x eh oa Intensity Units No normalization 0 01 0 02 0 03 0 04 0 05 0 06 Radial q 7 Counters Image Operations Exposure Secs eemg lo Counts 282208 B Stop Counts base oo Transmission 0000149053 Scaling Factor ooo Transmission SAXS Exposure i The Log file e displayed here Slits tad Record Full Status Normalization entries 176
12. er Shutter Enable is Green on the Facility Status Monitor call the Control Room ex 123 and request control of the Front End Shutter for SAXS WAXS ID13 e If the shutter will still not open contact local support staff pm pm pm mm pm pm pm pm pm pm pm mm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm pm zeg sci E EE mala em e EE E AE ui scm ia imma HE Je a r get de Ae VE e ef A ig E ee em rm re pm re ps re em re em pm e Fe e em re em re em Fe rm Fe re em re rm Fe rm Fe pm rem re rs re rs re ps re zi l Energy setting for undulator and DCM return to the set point automatically however this should be checked 5 e In SR13ID01 Energy Control shown to the right check that the Blue and Master energy fo de SS Green numbers agree E Undulator e If not check that the Stop Status is t rege Active RE N nm zi Harmonic C s E cleared If not press the Clear Aen unn es Wm button Eneray ban SET e Click the Green Move button above ean the green number for the Undulator 1 e Gap The undulator should now move t er 050 om to the correct position e If this fails click in the Blue area for the Gap type in the desired Gap and press Enter e If this fails contact the Control Room ex 123 or local support staff SR13ID01 IVU Beamline Control elected Control ee eT
13. esolved contact local support staff e Ensure that the correct Flea camera is selected in the Flea Viewer e Ensure that Start Video is depressed e Press the Restart Camera button e Close the Flea Viewer and reopen using flea_viewer sav from the desktop e Contact local support staff Cryocooler Alarm EPS Fault Motors not responding If the Cryocooler alarm sound you are made aware of an EPS fault or Motors on the beamline do not respond e g Sample Height not moving Version 1 2 05 05 2009 This section lists some common problems and suggested solutions for the SAXS WAXS beamline Try the suggested solutions in the order that they are listed If you are unable to resolve the problem contact local support staff Bug caused by a digital output signal that should be always 1 dropping to O If this happens all attenuators drop in to protect the detectors from over exposure and potential damage However this can occur in error and beam o Use the main optics control computer which is furthest to the right of the computers in the control area e If SR13ID01HU02IOC02 adl screen is not running it has 5 columns amp 8 1 rows of green buttons start it using the desktop icon OPI MEDM which is at the top left of the desktop and looks like a butterfly e In SR13ID01HU02IOC02 adl left click on Digital and left click on the first i button in the drop down list called Unidig 1 I O 24 or less e In
14. f scan points sues Ea EE SEES TS Positioner 2 a nppp ee ee 0 0000 Motor Selection _ p z ooo Se Positioner 2 l Move to this gt om 0 0000 EEN 0 0000 i Positioner 2 Heine 0000 Ho 0 0000 zm Scan start point iz stj Link biw Pos 1 amp 2 CE Grid Trajectory Positioner 2 Total no of exposures 10 Scan end point i Pssitioner i PV Monitor Set Start Move Scan Number of scan points Done Version 1 2 05 05 2009 7 0 AFTER INJECTION INTO STORAGE RING Twice a day at 8 00 am and 20 00 pm the Control Room will perform an injection of electrons into the synchrotron storage ring This is announced with the warning An injection into the storage ring will commence shortly and the notification An injection into the storage ring will now commence e The beamline Front End Shutter is closed You will need to reopen it e The Undulator Gap will be set to 10mm It will reset but needs checking Follow the steps below after injection and wait 5 minutes for the DCM to warm up before resuming data collection H e Await announcement that Injection into the storage ring is now complete e Wait for shutter control When control is returned to the beamline the Facility Status Monitor light PSS Master Shutter Enable will be green e Open the Front End Shutter also called Hutch A Shutter using the computer control our touch panel e If this does not work and if the Mast
15. group spokesperson and signed by all appropriate parties Submission must be via scanned email not via post or fax to the user office as soon as possible and well in advance of the experiment Australian Synchrotron travel funding will only support up to S people per experiment excluding Foundation Investor allocated ey i yoy Manual Page 6 Version 1 2 05 05 2009 2 1 CHEMICALS amp CHEMICAL SAFETY ze e e e e e e e e e e e e re e e e e re e e e e ee a e e e e e e e e re e ee e e e e e e e e ee e re e e e ee eee eee ete ee e e e re e e e e re e re e e e e e e e e e e re e rn e rn Cryogenic Safety i Liquid nitrogen will be may be made available upon request from local support Staff Safety glasses and gloves will be provided for handling the liquid nitrogen outside the hutch In the experiment hutch cotton gloves covered by nitrile gloves and safety glasses are required to handle liquid nitrogen Users are requested to provide their own cotton gloves A durable foam rubber dewar Spear Labs that holds 800 ml of liquid nitrogen is provided at the beamline They are easier to handle and safer than a low profile glass Dewar and a lower thermal mass causes less liquid nitrogen boil off when it is filled Chemical Supplies A range of chemicals and solvents are provided for users in the Chemistry Laboratory including Solvents Water Isopropanol Methanol Ethanol Acetone Chloroform a
16. ile Settings Help Image Control Motor Control Stat Video d Pause Video HOMERN C BARNEY S LENNY Cursor Position 320 240 Beam Cursor Position 204 204 Box Parameters Set Background seat Backgrounds Z Image estat Care ia CP Shutter Hra A i we ain Flea cameras are designated by names eg Homer The available cameras are shown in the top left of the window and the displayed view is changed by clicking on the desired camera name The SAXS WAXS Beamline User Manual Page 12 Version 1 2 05 05 2009 lr rs rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rr rm rm rm rm rr rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rs rs rm rm rm rs rs e Crosshairs Green crosshairs are fixed on the present display only Red crosshairs remain in a fixed position on all computers displaying the camera feed This allows the Red crosshairs to be used to mark the sample and beam positions on all computer displays while remaining outside the hutch he Red beam position cursor may be locked in osition using the Lock button in the viewer o Image Zoom Magnification In addition to manual optical zoom digitally zoom may be used in the Flea Viewer Note that this yield poorer resolution Alt Left Click zooms in i Alt Right Click zooms out Motor Control By selecting
17. k hutch Shutter must be closed Security Lock Security Lock 09 29 17 17 08 2007 SYSTEM PAGE Note The touch screen of the Control Panel requires a relatively firm touch to register Version 1 2 05 05 2009 2 0 BEFORE YOUR EXPERIMENT Prior to your arrival for your experiment at the Australian Synchrotron the following steps must be completed liaising with the User Office For further information please contact the User Office user office synchrotron org au 1 Return of Experiment Authorisation Form i 2 Booking Safety Training for Users can only be completed after return of experiment authorisation form 3 Travel and Accommodation Requirements 1 Experiment Authorisation Form The experiment authorisation safety form must be returned a minimum of 1 week prior to your experiment The User Office must be provided with a list possible of all users who will De attending the experiment and detailed information on all samples that you will be bringing User s not on the form wont be able to have safety training be issued dosimeter or access card All samples must be listed Please also note that if you are bringing any hazardous chemicals the relevant OHS assessment forms MUST be filled in and relevant MSDS for those chemicals attached otherwise ESA forms will NOT be signed off For oe in filling out the experiment authorization form please follow the link htt www synchrotr
18. ltiple Exposures with Movement or Delay Time This procedure will move the SAXS table to the correct height and will take exposures and move the sample following a program e In the top menu go to Acquire and select Move Expose le Select the Exposure Time in the drop down menu i e Enter a wait time in seconds for a delay between scans e Select the first motor in the Positioner 1 drop down menu le Enter the scan range and number of points in the scan press Import Select the second motor in the Positioner 2 drop down menu e Enter the scan range and number of points in the scan press Import Ve Select Grid for a raster pattern or Trajectory for a diagonal line i e Press the Start Move Scan button to begin the program Note For a 1D line scan select the motor in Positioner 1 only For a stationary scan with multiple exposures select none as the motor and enter a scan range This will collect data but not move ee Move Expose Sequence x I Exposure Time i Set up move expose sequence drop down menu i xposure Setup Motor Selection Positioner 1 Starting number D i o000 Daes nessa can ini ate 0 0000 Positioner 1 GEET SE 0 0000 Scan start point NN SE 0 0000 TAN A a fao 0 0000 1 Move to this gt 10 000000 Positioner 1 i 0 0000 0 0000 Scan end point a Ae 0 0000 Go KEE 7 ia i 0 0000 Positioner 1 i mn iges ae 0 0000 l Number o
19. mm may be readily mounted using sample mounting plates brackets provided on the beamline Additionally Samples in capillaries may be mounted vertically or horizontally in For larger samples or for a specific sample mounting please contact support staff and a custom mounting can be readily arranged Sample Rotation Tilt and Translation In addition to the translation of the sample stage a rotation stage and a 2 dimension tilt stage rated over 100 ko are available to provide sample movement alignment Additional linear stages rated at 90kg or 10 kg are also available for mounting on the sample stage if D is preferable to move the sample without moving the sample stage Sample Alignment Visual alignment using the flea network cameras detailed in ee section 5 2 is the most common alignment s procedure Samples are aligned against an ee on screen cursor set at the known tested beam position This procedure provides a EH precision of better than 10 um however p samples may also be aligned directly at the beamline end station or by a beam scan across a sample if required Version 1 2 05 05 2009 9 0 FLEA CAMERAS Observation and alignment of a sample on the beamline is performed using video cameras viewed over a network This is of particular use when the experimental hutch is secured as sample movement orientation and alignment may be directly monitored It is also
20. nd Toluene are also available in smaller quantities i Acids Hydrochloric Sulfuric Nitric Acetic e mae EE E EE EE EE E Chemical Safety and PPE Nitrile gloves laboratory coats of a range of sizes and safety glasses are provided at the chemistry laboratory Personal Protection Equipment isi mandatory when in the laboratory and when handling lt t Chemicale Users are expected to follow safe handling 4 procedures for their samples and when using chemicals during sample preparation Before arriving at the facility for their experiment users are required to supply a Material Safety Data Sheet for any and all chemicals they intend to bring into the facility Solvent waste containers chlorinated water soluble non water soluble are provided in the chemistry laboratory Users are responsible for the safe disposal or removal from the Synchrotron site of their own chemicals and samples i n Version 1 2 05 05 2009 3 0 USER RESOURCES SUPPLIED rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rm rs rm Laboratory Supplies The chemistry laboratory is located opposite the SAXS WAXS beamline and proximity badge access may be arranged through
21. on a jack rated to over 200kg and precision adjustment is facilitated in three dimensions Stages are also available for precision rotation and tilt control while a water bath and temperature controller is User Lounge A lounge has been provided for users to rest relax and eat in it is located on the ground floor Tea coffee and mugs are freely available in the user lounge and a vending machine is available with food and soft drink Fridges are also available to store food brought into the synchrotron as there is no cafeteria at the facility Users are requested to be considerate to others and dean up after themselves Food is not encouraged at the beamline however beverages are permitted at the SAXS WAXS beamline i User Manual Page 8 Version 1 2 05 05 2009 4 0 BEAMLINE OPERATION 4 1 CAMERA LENGTH ENERGY amp Q RANGE Considerations Camera length and energy can be changed during an experiment if required however when choosing or requesting a camera set up a range of factors need to be considered The camera length and X ray energy both effect the observable Q range of the instrument as shown in the table below Camera lengths of 650 950 1250 1550 3000 3300 and 7000 7300mm are available using different nose cones for a 300mm adjustment A 330mm length is also available but requires additional set up time Energy may be selected in the range of 5 20 0 KeV The absorp
22. on org au content asp Document ID 5309 2 Book Safety Training Safety training and a test are required to access the experimental hall hutches and laboratories This test must be done bi annually to ensure users are up to date If you have not previously used the beamline or laboratory required for your experiment a beamline induction must be done with the beamline scientist before access will be authorised Before arriving at the Australian Synchrotron review the documents below http www synchrotron org au content asp Document_ID 5162 There is a 1 2 hour onsite safety induction to complete upon arrival at the Australian Synchrotron This must be arranged at least one week before your experiment To organize send details of all users attending the experiment full name e mail address and contact telephone number for each team member to the User Office and note when you would like to do the training 3 Travel and Accommodation Interstate and international users may wish to apply to the Australian Synchrotron for travel funding see link below Accommodation is available for all users and will be booked by the User Office but users must arrange book their own flights and or ground travel http www synchrotron org au retrievemedia asp Media_ ID 5416 In order to apply for funding from the Australian Synchrotron an application for travel funding form must be filled in by the
23. orrect height and take an exposure for the time selected e Select GANG Exposure using the check boxes below the radially averaged profile e Select the desired scan length from the Expose drop down menu e Click on the Start Action button x Acquire Setup for MAR165 Detector Data Collection Multiple Exposures No Movement This procedure will move the SAXS table to the correct Acquisition Times height for transmission and exposure and will take poose Time Guo zD exposures as programmed onmands feted P Transmission Secs fi 0 0000 CCD Directory Setup As seen from here Browse C data day2 As seen from CCD server Shome marced data day2 To Program e In the top menu go to Acquire and select Set Up e Select Auto from the Exposure Time drop down menu e Enter commands separated by commas in the box t transmission eN is an exposure for N seconds e e g the program t el e5 will take a transmission CCD Software Settings _Initialize scan a 1 second exposure and a 5 second exposure CCD Chip 2048 2048 ob PY Prefix fi 3MARCCD1 cam1 Image Corrections F Apply spatial correction Data Collection e Select Auto as the scan length from the Expose drop down menu in the main SAXS15 interface e Click on the Start Action button Je Apply dark correction IV Apply flood correction Version 1 2 05 05 2009 Data Collection Mu
24. possible to fix crosshairs to mark a position on one or all monitors receiving a camera feed zoom in move the sample using a camera display and set an array of sample positions using markers on the camera display Fixed Cameras For sample alignment a Flea camera with a high magnification lens is maintained in a fixed orientation The camera uses a mirror in the flight tube to provide an upstream view of the sample position coaxial with the beam This allows direct observation of the beam position and highly reproducible sample alignment with a known beam position H designated by an on screen cursor Movable Cameras In addition the fixed camera for sample alignment cameras are available to be positioned as required These cameras allow additional views of the sample position orientation and movement during alignment and measurement This further facilitates rapid sample alignment and is of particular use for the measurement of mobile samples and Tor data collection regimes including sample movement i Version 1 2 05 05 2009 5 1 FLEA VIEWER Changing between multiple camera feeds placing cursors and all other functions of the flea cameras are controlled using the Flea Viewer program detailed below If necessary the Flew Viewer program may be reopened using the file on the desktop and Click Start Video IO x Al Flea Viewer F
25. st 2 iti 17 282208 0 347983 0 Gin Lan 19 23 24 28 2009 UDEF1_2PV1 2345 1 5002 00000 10000 13 900 39 700 27 951 4 8958 4 Selection of a Transmission scan Or Start Action button used to SAXS Exposure SAXS Calibrate is not i begin data collection once the yet implemented desired scan type is selected SAXS15 Manual Documentation for the SAXS15 software is available at the ChemMat CARS website URL below and is also available at the SAXS WAXS beamline The unmodified SAXS15 software may also be downloaded from the website http cars9 uchicago edu chemmat pages swsoftware html Version 1 2 05 05 2009 6 1 STARTING SAXS15 During your experiment it may be necessary to start or restart the SAXS15 software controlling the MAR detector e g if the software freezes or crashes To start SAXS15 follow the steps outlined below e Ensure SAXS15 if previously running is closed e Ensure IDL if previously running is closed e Open IDL using the shortcut on the desktop e Click to continue e When asked which Workspace to open click OK e Inthe Command Line type saxs15id_3296 epics e Select No when asked about the run mode Once SAXS15 is running you will need to set up the Log File and Parameters File in order to begin collecting data Log File e Inthe top menu go to File e Click on Get Scan Log e Find your Log File C Data Your Directory log e Select the log file
26. ter I 512 al gt l M Auto Gain I I I I I Start Video Sege I Pause Video I l Ze HOMER I C BARNEY I I the sample stage e The SAXS table is positioned to allow direct viewing of the sample in the flea viewer i e With the Red cursor still marking the position of the beam the sample stage is moved to place the desired Sample position at the crosshair ie It may be necessary to check the beam position with a YAG crystal if the beam has moved e g after changing X ray energy after injection or 3 after a tweak of the 2nd crystal pitch in the DCM e The sample may be positioned by moving the sample table motors directly or by using the Motor Control feature of the flea viewer i e Additional flea cameras can be readily set up as required to provide i additional views or displays of the sample to aid or further hasten sample alignment Version 1 2 05 05 2009 9 3 SONY NETWORK CAMERA In addition to the range of Flea cameras provided on the beamline a Sony Network Camera is available which provides a broad controllable view of the SAXS WAXS beamline It provides the ability to remotely monitor the beamline in a broad picture or a narrow area e g an equipment readout as required It is accessed via a bookmark in Firefox on the beamline computer Control Button When starting the view Movement Controls These buttons are used to move from the Sony network camera Control ithe camera view
27. the 24 channel digital IO screen click the Channel 23 to Low then click it to High It must toggle to low and must be left on high If unsure do this a few times Toggling Low amp High is what fixes the output signal o Make sure that the Top Level control screen for the optics is running it has the picture of the full beamline optics on it If not double click on the i desktop icon SAXS OPI located at the top left of the desktop e In the main Top Level control screen click on the Filters button Make sure all attenuators are set to the IN position on the Filters screen o On the Top Level Screen click on the button marked EPS near the top of i the screen in the middle This will open up the EPS screen o In the EPS screen there are buttons that look like the Filters screen for controlling the attenuators Although looking similar the button control properties are subtly different In the EPS screen change all attenuators i to the out position All attenuators on the EPS screen should remain out and not drop back in by themselves You MUST set XIA2 Ch 4 to out on the EPS panel K Look at the Filters screen You should see all attenuators out except the one at the bottom right XIA2 Ch4 which acts as the shutter Try taking a i SAXS exposure which should work normally i e the shutter will open and close under control of SAXS15 and attenuators should not drop in e If this fails and a SAX
28. tion of the sample and available flux for different incident energies should also be considered If you are uncertain of the Q range camera length or X ray energy you require please contact support staff prior to your experiment A t 0 002 0 05 0 003 0 06 0 0035 0 07 0 0043 0 089 20 and d spacing For users more familiar with considerations of instruments in 20 or d spacing a quick reference for 250mm and 7000mm camera lengths is provided in the table below 20 range d spacing range 20 range d spacing range 0 35 7 deg 12 250A 0 03 0 67 deg 130 2700 15 KeV 0 35 7 deg 6 5 135A 0 03 0 67 deg 70 1450A Version 1 2 05 05 2009 4 2 SAMPLE MOUNTING Sample Position The sample position pictured to the right consist of an adjustable plate mounted on a jack The jack is rated to approximately 500 kg and is moveable in three dimensions with 2 um precision Equipment and stages may be readily mounted at the sample position and fixed in place using the hole pattern for 6mm bolts For particularly large equipment Or sample environments the entire sample stage assembly may be moved and support staff should be contacted if this is required Sample Mounting A steel breadboard is used at the sample position to allow positioning of sample holders and allows rapid installation of different sample mounting arrangements Small solid samples 0 1 40
Download Pdf Manuals
Related Search