Bruker D8
Contents
1. option Append except for the first frame Merging the different ranges e Load the raw file in the program merge e Select Do it The program creates a merged file named merge out e Rename this file with a raw extension You can also do the merging inside the Gadds program by selecting Special System and writing merge in the command field Printing a X ray diffractogram e Open the raw file with the program EVA e Print the diffractogram EVA has a lot of features To learn about it play with it and read the software manual2. Bruker D8 GADDS User s Manual e Responsible Fabio Ziircher tel 642 2148 or 528 4763 email zurcher socrates berkeley edu e Diffractometer s mailing list d8gadds_dif socrates berkeley edu e Diffractometer s web page _ http theanvil cchem berkeley edu gadds e Computer bragg cchem berkeley edu username gadds password e X ray source CoKa A 1 79026A If you have any doubt ask Fabio before improvising Important Each time you touch the diffractometer be gentle especially with the microscope collimator detector or beam stop If the shutter is open never open the diffractometer s windows When you are moving the goniometer manually or with the computer beware of collisions Before starting a measurement always check the alarm lights Do not log off the computer The generator operating power is 45kV 35mA The generator sleeping power is 20kV 5mA Measuring a Powder X ray Diagram e Open the program Gadds if it is not already open e Set the generator s power to the user s setting 45kV 35mA Before starting the measurement always check the generator s power Collect Goniometer Generator Create a new Project e Select New under the ProJect menu Example create a project called uffa in Fabio s personal directory Options for ProJect New Note you must create the new project in your personal directory by writing D frames username pr
3. and read the software manual Integrating the Frames e Select File Load to load the frame If you have measured a blank frame you can subtract it from the measurement s frame in the Load window Example the blank frame uffal_2_000 gfrm will be subtracted Scale factor N from the measurement s frame uffal_1_O00 Options for File Load D frames Fabio uffa uffal_1_000 gfrm Pe sos a D frames Fabio uffa uffal_2_000 gfrm fa oo 8 e Select Peaks Integrate Chi Choose 3 Normalized by solid angle faster or 5 Bin normalized slower in the Normalize intensity field and the desired Step size e Using the 2 3 4 buttons and the mouse you can adjust the size and position of the frame s sector that you want to integrate The Enter button starts the integration e When the integration is complete save the raw file Always choose the DIFFRACPlus format The Write window comes automatically when the integration is completed but you can save the raw file again later by selecting Peaks Integrate Write INTEGRATE ZWRITE options x Title Uffissima File name fuffa raw l Format DIFFRACplus E Append Y N Scale factor fi 0 5 Cancel Note If your measurement has different ranges more then one frame you have to integrate the different frames separately You should assign to 20 Start the same value you used as 20 End in the previous frame Save the raw file using always the same name but select the
4. e the symbol for the x y z positions current value The usual Scan Axis is 1 2T 20 The typical values are 0 for capillaries and 15 for reflection measurement For transmission measurements select Coupled in the Scan Axis field which stays for a 20 0 scan W 20 2 2 Option multiple samples e Select Collect Scan PickTargets You enter in the manual mode e Center the first sample in the microscope using the manual control box e Press Esc on the computer to exit the manual mode and add the position to the targets list e Repeat this procedure until you have centered all your samples Beware of collisions e With Collect Scan EditTargets you can check and edit the targets in the list e Select Collect Scan MultiTargets Example using the following options you will measure the targets in the list collecting three frames for each target The frames are collected at 20 30 40 and 50 is fixed at 15 The frames names are uffal_X_OOY gfrm with X target number Sequence and Y frame number in this case 000 001 002 Frames B 2Theta 30 0 Omegafi5 0 Philo chifo 0 Scan Axis h r S Frame width foo Seconds frame 00 Job name atta Title Uffissima Sample name utta Sample number Max display counts 31 M Realtime display M Pre clear Sequence of starting run if S Sequence of ending run 999 gt Mode step x l Rotate sample Note all the targets are measured using the same
5. ojectname in the field Working Directory The program will create a new subdirectory called projectname in the username directory The projectname directory should contain a file named gadds _nc where project s preferences are stored You can also use an old project ProJect Load or read an old gadds _nc file Edit Configure Read e Check whether the numbers on the gadds window are correct and whether the program loaded the right detector s distance flood field correction and spatial correction Moving the Goniometer e Within the program gadds Select Collect Goniometer Drive e Using the Manual Control Box Select Collect Goniometer Manual and press Shift F1 on the Manual Control Box Commands on the Manual Control Box 1 20 5 X 2 6 3 not in use de 4 x not in use TL to move drive speed Emergency stop when driving the goniometer press any key on the keyboard Mounting the Sample e If you are measuring capillaries set the collimator in the standard position with the pin in the hole and mount the beam stop e If you are measuring plates set the collimator at a higher distance with the pin outside the hole and do not use the beam stop Be careful that the direct X ray beam does not hit the detector e Mount the sample on the XYZ stage e Move the goniometer angles 28 and at the position where you want to start the measurement Beware of collisions especially with the beam stop sample holde
6. options angles time It is very useful for running several samples plus a blank X ray diffractogram which can be used for subtracting the background caused by the air scattering 3 Other Options e EditRuns MultiRuns you can program several runs with different measuring angles but only one single target CoupledScan you can perform a 20 0 coupled scan W 260 2 using the area detector as a point detector e Add you can measure one frame at the current and fixed angles for a specified collecting time Note that the frame is not automatically unwarped therefore you have to select Process Spatial Unwarp and save the unwarped file as gfrm To interrupt a measurement press Ctrl Break If a measurement is currently running you can not use the program Gadds Open the program Gadds Offline instead Analyzing the Frames The frames are already unwarped except if you use Add to collect the frame e Select File Load to load a frame e Select Analyze Cursors Conic to check the 20 angle of a reflection e Select Analyze Cursors Pixel to check the intensity measured on a pixel e Select Analyze Graph Write to save the graphics in the frames not the frame itself for further use e Select Analyze Graph File to open a saved graphic on a frame The program Gadds is also able to calculate the percent crystallinity the stress of a probe and many other properties If you want to use these cool features check with Fabio
7. r or collimator 1 Option single sample e Select Collect Goniometer Manual e Center the sample in the microscope using the manual control box e Close the diffractometer s window The alarm light should stop blinking e Select Collect Scan SingleRun Example using the following options you will measure two frames uffa0_1_001 gfrm uffa0_1_002 gfrm for 10 minutes each with 20 as Scan Axis and 15 The first frame will be measured at 20 30 the second one at 20 50 Frame width 20 SCAN SINGLERUN options x Frames 20 Seconds frame fi0 00 0 2 Theta 30 000 deg Omega 15 000 deg Phi0 000 Chi 90 000 3 066 mm 3 876 mm Z 9 205 mm Aux 0 000 Scan Axis h r S Frame width 20 00 Mode stee T Rotate sample Sample Osc None Amplitude 0 Frame header information ne ae ee oo Title Utfissima a Sample name Ro Sample number ss Weed etd aR nad SE ase T d Ae i resaenenanennsetenerseeeennsesnenasentsae tesa seeteseseeresusisaeensvarsentasentvanereiegesiesessebrsanetssessiteaestesrsestesesentsseeitsseberansrhaserevsnnsninsunersesesirsosesnrsne tenesentesestisweestesesuteserstarsstvsenersnseetyseseeersneeTseestts J _ Filename generation O O re Job name uffao Run fi Frame 001 First filename pila ee zZZE Max display counts 31 M Realtime display gilasiuisakalueaskivedlickanl Pre clear M Capture video image Fitesendenacanvnonie toxieabonn Note Us
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