Operating the Siemens XRD Diffraktometer D5000
Contents
1. ES EP ol he 15408 Os ei Puen e einer l I oor Oe FV ee JU gt E M z ill De p E rM nr re i nns A yif e Sus i T Taa Mi Wi j pete lim hod EIC Doc B ome eS BSR RS RRS RS Je RS Ss Be 3 Theta i 22 82 d 2 000 Courte 44 9 8 66 06 Ron 5534 O em Mon Ga zoo een dva mo axe dye suse nam 32 8 8 8 9 8 10 8 11 8 12 Potential Sources of Error and Uncertainty Criteria for recognizing and evaluating potential sources of error and uncertainty will be indicated by the Procedure User s inability to obtain a quality image or to generate a semiquantitative or quantitative analysis within tolerance limits Acceptance criteria for quantitative analysis of Samples are based on acceptable analyses of appropriate standards Procedure Users may use as a general guide a value of two sigma That is if standard analyses are within two sigma based solely on counting statistics of the list or published values then the analysis is acceptable Procedure Users may define different acceptance criteria Equipment Malfunctions Malfunction of the Diffraktometer D5000 oystem is readily detectable by the Machine Custodian during operation of the instrument If a trained Procedure User has doubts concerning his her ability to detect equipment malfunction during operation of this equipment he she should consult w2. Clone il i Scan MM J 14 06 7 Cuevas raw d p Pattern 1 Save Ctr S Save As Import Close Ctrl W is b l Gurrent DIF Patt BE 5 8I PHP I0 TR mnn pm Pld TANIE MAR A h Print Ctrl P Gurrent Pattern as DIF file LXI CN LC i ae DES ERI Print Preview Preview picture as MebaFile 50 60 Page amp Printer Setup Bezier Gurve Print All Documents DEN TL l 1 C DIFFDAT1 7 Cuevas raw 2 C DiFFPlus Tutorial Lab6 eva 3 C DifFPlus 4UST_H raw 4 3D Rocking Curves EYA 5 C DIFFDAT1 Alexis Cruz RAW 6 C ADIFFDAT1 clc sand RAW 7 C DIFFDAT1 40calcite RAW 8 C DIFFDAT1 quimical4 RAW mr T 00g e 80 4 EE Fra Doct fe Cuevas I3 Cuevas E start e ad x o biffra Biuwmrr Biystatu Gysor s wi sor s Seva Cxorrro EST EDT METET 28 8 8 To save the graph open the EVA icon then click File option click Export and then click Current Scan Working Area Only and save it Note The program save the graph as a raw extension Aaen Nes hy Fan Sa nr unit Y unit Y scale s T Current WL Scan WE J 14 06 7 Cuevas raw Fixed 2 Theta Counts gt Linear 1 54056 Cu Pattem 4 Search Match Criterion Subfiles fi Favor Simple Patterns Inorganic 2 guts z Quality Marks Organic J fo Displacement Dual n yy ae i EEHITIJEZME NARRA A add 6D 70 S U
3. File Edit View Favorites Tools Help Back 3 Bsearch Gyrolders 4 Um GE X A E Address 63 DIFFRAC PLUS Evaluation A em fAbsorbX DBViewer DQuant E File Exchange PDFfSGsint Print Setup Raw File Read me DIFFRAC PLUS Exchange please Evaluation Select an item to view its description See also My Documents My Network Places My Computer 4 9 object s 3 87 KB ig My Computer Fa Doct A 7 Cuevas Fa 7 Cuevas E 2 Theta 32 509 d 2 75195 Counts 0 05 0 16 i stat ew x iw HO Goorrre iur Estatu Cusoes msor s Deva Srn Leme 3 47 em 30 8 7 11 Now click the Open option write a name for this file which translate to UXD source that could be open in another computer and format 8 7 12 To convert a RAW file into UXD file e n XCH Click Open button XCH displays the Open dialog box e Inthe Files of type list select Scan File raw e Browse to the folder containing the RAW file of interest select it and then click on OPEN 8 7 13 Click on UXD to convert into Exchange format UXD file I xcH J Guanajibo RAW 1 23 File view mares Help aeg ele el Cal Sr Z J Guanajibo RAW Diffrac Plus V1 01 File CADIFFDAT1XJ Fus e RAW Measurement time 29 Mar 2006 19 38 Number of Data Ranges in file 1 Location C DifFPlus es ig My Computer start e a3 x w 75 O il s
4. 8 6 3 8 6 4 8 6 5 Environmental Considerations Maintain the room temperature between 17 C 62 F and 26 C 78 F at a gradient less than 0 5 C hr and a fluctuation of no greater than 2 C Relative humidity should not exceed 80 and should be no less than 20 Ensure that the heat produced from the generator spectrometer computer and vacuum pump is adequately dissipated by ventilation or air conditioning and located so that the air flow is not directed at the instrument A clean dust free environment is also necessary Avoid the direct sunlight to XRD machine Chiller must be turn on 5 to 10 minutes before of the operating the XRD machine at pressure of 60 80 psi and a temperature of 65 F On the panel of the left side in front of the XRD machine Turn on the green switch of ON and OFF Turn the key Press the yellow button Now on the panel of the right side of the XRD machine pull out the drawer and then Press Shift button Press X ray button Press 1 button Press Enter button Back on the left side of the panel in front of the XRD machine Press the green button then an X ray indicator will turn on 15 8 6 6 Aspects of X ray tube design and operation A new tube is about 3 000 and should last several thousand hours 8 6 6 1 Increase the current mA and the voltage kV 10 units by 10 units waiting 1 minute between each rising to get the optimum values of 40 mA t
5. amp Computational Geo Sysor s W SOP Siemens XRD ubiffrac Plussi1 PDifractometer 1 xi CS SENS 10 31 am 8 7 4 A Tool Box window will appear or find it at the View option 26 2 E A Doci PQ File Edit view Window Help Diesmal r aoe Ble Ne sa Galena Salt ts Zoom 4 Screen A unit Y unit Y scale Slis Pat Cument wL Scan l 1 Segment v 2 heta v Counts Yf Linear v Fixed Y None Pattern xf Scan Pattern Peak Area Label Level E tmx amp ug cmm mA Sample name File name Scan Type Start End 5 Fen Gray All Except Current Items Selected None Aj Backgnd PeakSearch Strip KA2 Fourier Smooth X ffset Displacem Y Scale Aberrant Add Subt v Subtract from Scan Enhanced Default i Curvature Bezier Replace T 1 Threshold Append For Help press F1 A start S GB x pw Gpoiffraction Basics W s0P Siemens xRO CuDifracPlus 1 Seva Doct 419M 8 7 5 In this Tool Box window press Scan option to replace the background the Ka and Smooth the graph by clicking the Background Strip KA2 or Smooth option and then clicking Replace button 8 7 6 Press Pattern option and with the Search Match option to match and identify the elements and compounds of the sample 27 ER EVA 7 Cuevas EVA File Edit view Window Help Degli Zoom Screen L WL Scan MD
6. J 14 06 7 Cuevas raw H f1 Segment T 1 54056 Cu Pattern _J Search Match x Criterion r Subfiles fi Favor Simple Patterns Inorganic Seisei r Quality Marks Organic o Displacement Dual E fi s TU TEC NT g d AA F 4 J Mineral V L M M ete PU nda 6D EUM 80 r Chemical Filter Hio He Li Be Cc Ne Nal Mg Si K Ca Sc Ti V Ni Cu Zn Rb Sr Y Nb Pd Ag Cd Sn Cs Ba La Hf Ta Pt Au Hg Ph Fri Ra Ac Lanthanides Ce Sm Eul Gd Tb Dy Ho Lu Toggle All Th Pa Np Pu Am Cm Bk Cf Es Fim Md Nol Ln Scan W 14 06 7 Cuevas raw Pattern J String Main Database Max Results MASTER 50 4 F add User Database to search Insert in Current Document v Read Save Default Search E eae 20 Experimental MAP Skip Non Ambient v d multiplied by 1 B M G M n e Doct Fe Cuevas lies 7 Cuevas E 2 Theta 48 796 d 1 86477 Counts 33 6 Y 104 90 NUM PAstart e aune Cbiffrac P ga uvrime Status p Sysor s W SOP Sie Sheva rc XDIFFDATI OBR 3 15PM 8 7 7 Or search by name R EVA 7 Cuevas EVA r File Edit view Window Help New Ctrl N m amp amp lm Open Ctr o
7. gt For Help press F1 Dr Pa Location C DiFFPlus 452 bytes Ia My Computer A start B x wl gt Computational Geo ysor s W S0P Siemens XRD CyDiffrac Plus 1 BR unten Edit Sep HS 10 54 0m 8 6 17 Or select and click on Qualitative Extended to edit and set up the parameters such as e Comment e Starting Angle e Stopping Angle e Step Size usually 0 01 for more precision and 0 02 for a faster run Time Step e Scantype usually locked couple e Scanmode usually continuous 19 M wr Diffrac Plus 1 2r File E en Favor Tools Help iL ee 9 xil sd Curodes C96 DE X dl E Addre ALALLE Edit DQL We Measurement Setup iew Help Em Ne i f Edit Qualitative Measurement Extended Instructions intenance Comment Bf ness Scantype locked coupled v Scanmode continuous User Task File Si Browse Default Scan Parameters 2Theta Start ioo deg Stop ano deg Step size pozo deg Time Step 1 00000 Theta Start 5 0000 deg Stop deg Step size deg Delay time nono s Steps Scan time Default Fixed Axis Settings 27 00000 dea T O00 chi 00000 dea Phi 0 0000 deg A pon mim Y pono mtm Z 0 00000 mm Auri pono degormm Aus z po0000 degormm Aug 3 poo deg or mm Default Slit Settings Divergence slit 1 0000 deg Synchronuous rotation on Range Entries Antiscattering slit 1 0000 deg Rotation speed pm o
8. Identifier Revision Effective Date Review Date University of Puerto Rico SOP 001 2 07 12 2006 03 26 2007 Geology Dept Document No EXACt 001 di Lg J Author Miguel A Santiago Rivera Department of Geology UPR NSF Earth X ray Analysis Center EXACt Standard Operating Procedure for Operating the Siemens XRD Diffraktometer D5000 UPR NSF Earth X ray Analysis Center EXACt UPR Mayaguez is an affirmative action equal X Ray LABORATORY opportunity employer is operated by the University of Puerto Rico DEPARTMENT OF GEOLOGY F 304 Geochemistry Facilities at Physics Building University of Puerto Rico Mayag ez Campus Revision Log Revision Effective Prepared By Description Affected No Date of Changes Pages M July 12 2006 Miguel Santiago All New Procedure 2 September 20 Miguel Santiago Warning in the 2006 Procedure 8 6 6 X rays Warning for Pregnant and Cancer patient 8 0 Procedure Operating the Siemens Diffraktometer D5000 Table of Contents 1 0 2 0 3 0 4 0 9 0 6 0 7 0 8 0 9 0 10 0 PURPOSE SCOPE TRAINING DEFINITIONS RESPONSIBLE PERSONNEL THEORETICAL BACKGROUND EQUIPMENT PROCEDURE RECORDS REFERENCES Oo fF A A AXA 11 34 34 Operating the Siemens Diffraktometer D5000 1 0 PURPOSE This procedure provides instructions for the operation of the Siemens Instruments incorporated Model Diffraktometer D5000 x ray diffraction system The D5000 mode
9. SA Chemical Filter He B C N O F Ne ASI S Cl Ar Ca Sc Ti V Cr Mn Fel Co Ni Cul Zn Gal Ge As Se Br Kr Rt Sr Y Zr No Mol Tc Ru Rh Pa Ag Cd In Sn Sb Te _ Xe Cs Ba Lal Hf Ta W Re Os Ir Pt Au Hg TI Pb Bi Pol At Rn Fr Ra Ac Lanthanides Cel Pr Nd Pm Sm Eu Gd Th Dy Ho Er Tm Yb Lu Toggle All Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Ln gt Scan EB I 14 06 7 Cuevas raw Patten t String Main Database Max Results MASTER 50 a F add User Database to search Insert in Current Document v Read Save Default sese apes ae ee aye Experimental MAP Skip Non Ambient V d multiplied by 1 4 J ER NER a Se SLAP RECS NE NN ON RS ER d Fa Doct B Cuevas PB 7 Cuevas E 2 Theta 48 796 d 1 86477 Counts 33 6 Y 104 90 NUM A PAstart e aunoa Cubiffrac P Bitur amp Status D CysoP s W 50P Sie Seva rc CDIFFDATI Lee 315m 29 8 7 9 Go to the Diffrac Plus Evaluation to save on an open extension such as xls extension 8 7 10 For Converting RAW Files to UXD Universal X ray Data which allow you to open the file and display its contents in others computers software such as Microsoft Excel etc e Click on File Exchange A EVA 7 Cuevas EVA Id amp DIFFRAC PLUS Evaluation D
10. X ray Electromagnetic radiation of very short wavelength 0 01 to 100 nm produced when an electron hits a piece of metal in an evacuated tube XRD X ray diffraction The atomic planes of a crystal cause an incident beam of X rays if wavelength is approximately the magnitude of the interatomic distance to interfere with one another as they leave the crystal XRD Siemens Diffraktometer D5000 system The system includes a chiller to control the temperature Driffac Plus software and PC to collect the data 5 0 6 0 RESPONSIBLE PERSONNEL The following personnel are responsible for activities identified in this procedure 5 1 Scientific Instrumentation Specialist 5 2 Faculty Member 5 3 Researcher 5 4 Student Participant THEORETICAL BACKGROUND 6 1 X Ray Diffraction X ray crystallography is a technique in crystallography in which the pattern produced by the diffraction of X rays through the closely spaced lattice of atoms in a crystal is recorded and then analyzed to reveal the nature of that lattice This generally leads to an understanding of the material and molecular structure of a substance The spacing in the crystal lattice can be determined using Bragg s law The electrons that surround the atoms rather than the atomic nuclei themselves are the entities which physically interact with the incoming X ray photons This technique is widely used in chemistry and all related science to determine the structures of
11. an immense variety of molecules including inorganic compounds DNA and proteins Cea hector KBfilter diaphragm Aperture diaphragm Scattered radiati diaphragm N K a 1 a 4 Lm i b xa bam e Measuring arc ig 8 Glancing angle 28 Diffraction angle a Aperture angle Diffractometer beam path in 6 29 mode 6 2 Bragg s Law n 1914 Bragg developed a law which defines a diffraction relationship between the wavelength of an incoming ray and the d spacing of a diffracting crystal Bragg s Law n 2d sinO where n the order of reflection wavelength of incident ray d interplanar spacing of the crystal 0 angle of incidence and reflection of incident ray This is the principle under which the wavelength dispersive detectors operate 6 3 Powder Method The powder method is used to determine the value of the lattice parameters accurately Lattice parameters are the magnitudes of the unit vectors a b and c which define the unit cell for the crystal e f a monochromatic radiation of a single frequency x ray beam is directed at a single crystal then only one or two diffracted beams may result e f the sample consists of some tens of randomly orientated single crystals the diffracted beams are seen to lie on the surface of several cones The cones may emerge in all directions forwards and backwards L Front reflections SN e A sample of some hundreds
12. d state synthesis In addition porcelain is a porous material and difficult to clean Agate a form of quartz is usually the material of choice but there are also other alternatives such as the Diamonite set shown above 12 In a typical solid state synthesis the reactants are placed in a mortar and ground by hand with the pestle Acetone or an alcohol is sometimes added to ease grinding Grinding is continued until the mixture is homogeneous the particles are no longer getting smaller and the solvent has evaporated With good technique powders with an average diameter of 10 microns 10 cm can be prepared If one has many samples to prepare and each requires frequent grinding or one has very large samples this method of particle size reduction becomes very tedious and physically taxing In this case a better solution is a machine called a ball mill which automatically grinds samples 8 2 2 Ball Mills It is also known as centrifugal or planetary mills are devices used to rapidly grind materials to colloidal fineness approximately 1 micron and below by developing high grinding energy via centrifugal and or planetary action An example of a four station planetary mill is shown below To grind a sample in this device you should already have reduced the particle size to less than 10 mm using a mortar and pestle if necessary Place your material in one of the bowls shown in the lower right and then add several balls shown i
13. der the UPR NSF Earth X ray Analysis Center EXACt quality program may follow this standard operating procedure SOP for XRD analysis May use their own procedure s as long as the substitute only if meets the minimum requirements prescribed by the UPR NSF Earth X ray Analysis Center EXACt Plan or are better in the performing and have been approved by the Director of the Department of Geology UPR Mayag ez Campus before the commencement of the activitie s Note UPR NSF Earth X ray Analysis Center EXACt personnel may produce paper copies of this procedure printed from the controlled document electronic file However it is their responsibility to ensure that they are trained to and utilizing the current version of this procedure The author may be contacted if text is unclear Deviations from SOPs are made in accordance with Department Director approval and documented in accordance with the GLP s WARNING X rays equipments may produce radiation out of the equipment Pregnant may risk in injury to the unborn child and or may interfere with the treatment for cancer patient If you are pregnant or cancer patient consult your physician before to use and or be exposed to x rays equipments 8 1 Introduction The XRD Siemens Diffraktometer D5000 Purchase Date month year Siemens Service Serial Number 001333 and UPRM Property Number 059933 allows the determination of crystalline structures and the identification of inorganic crystall
14. er A device which selects x rays of a specific energy traveling along a specific axis Two channel cut germanium crystals are mounted as periscopes in opposition The radiation diffracts from the first surface to the second where it diffracts again with direction unchanged but position displaced by the projected width of the channel The second crystal reverses the displacement so the beam direction and position are identical to the original beam The crystal lattice spacing in the monochrometer is effectively the metric standard to which the sample is compared Powder Diffraction X ray powder diffraction finds frequent use in materials science because sample preparation is relatively easy and the test itself is often rapid and non destructive The vast majorities of engineering materials is crystalline and even those that are not yielding some useful information in diffraction experiments The pattern of powder diffraction peaks can be used to quickly identify materials and changes in peak width or position can be used to determine crystal size purity and texture Reflection Sometimes used as a synonym for diffraction There is a big difference however in optical reflection the direction of the reflected beam depends on reflector orientation In diffraction the intensity of the diffracted beam depends on orientation but the direction is fixed in the coordinate system of the incident beam SOP Standard Operational Procedure
15. f ranges h Detector slit o Electronics Oscillations Temperature Scintillation fi of Osc set o cor AL pa Location C DiFFPlus 452 bytes e My Computer A PAstart a B x w al amp Computationa E50P s il soP Siemens EJ Diffrac Plus 1 Bor UNTITLED E Entire CS aS EF 11 09 am 8 6 18 When exit clicks save as to save your set up on a file 20 8 6 19 Back on the Diffrac Plus window click the Job Measurement lolx j File Edit View Favorites Tools Help Back search Gyrolders 3 G3 GE X A Ea Address a Diffrac Plus 1 C m o m Config DIFFRAC PLLIS DQuant EditDQL Environment Immediate Diffrac Plus 1 Evaluation Measurement Measurems Maintenance gt in E Immediate Measurement XS M Shortcut vice ter PDFMaint Service Status Display Uninstall Location C DiffPlus Contact Diffrac Plus Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal Location C WpiffPlus 448 bytes LE my Computer Astart 4 ae w amp Computational Geo ys0r s dl SOP Siemens XRD Sopitfrac Plus 1 diffractometer 1 sl come 10 31 AM Gh amp Diffrac Plus 1 cx i F Fie Edt view Favorites Tools Help 7 Back gt t Search Folders AsO X uc Es amp d e File Edit Job Option View Help Bema 5 viza aiv mieu JOB Meast Shortcu
16. flat Note XRD samples should be well ground in a mortar and or pestles This creates a uniform particle size and ensures that all possible crystallite orientations are present in the sample A special problem that can arise in sample preparation is called preferred orientation which usually occurs with rod or plate like crystals For example plate like crystals tend to lie flat on the sample holder very few will have a perpendicular orientation As there is no longer a random orientation of crystallites some of the x ray reflections that would be expected are unusually weak or missing altogether 8 2 1 Mortars and Pestles A mortar is a vessel in which substances are ground or crushed with a pestle A pestle is a tool used to crush mash or grind materials in a mortar In solid state chemistry a mortar and pestle is often used to prepare reactants for a solid state synthesis the ceramic method Mortars and pestles come in a variety of shapes and sizes A few of these are shown below On the left is a typical porcelain mortar and in the middle is an agate mortar and pestle set A Diamonite synthetic sapphire set is shown on the right The kind of mortar and pestle used in the preparation of a solid state material is very important If the sample being ground is harder than the material comprising the mortar significant contamination of the sample can be expected For this reason porcelain fired clay is not typically used for soli
17. he grinding unit material can be a complication 8 3 Selection of Standards The Procedure User may employ standards traceable to National Institute of Standards and Technology NIST formerly National Bureau of Standards NBS or well characterized materials published in credible technical journals and widely used by microanalysts for calibration of quantitative X Ray analysis routines Procedure Users may use their own standards from other sources for specific applications but must document the basis for usage of these standards in their notebooks For example reagent grade NaCl may be used as a CI standard by stating the material source and noting the stoichiometric nature of this material even though it is not NIST traceable 14 8 4 Sample Insertion and XRD D5000 Operation Detailed operating instructions for the XRD D5000 system are given in the XRD D5000 and DIFFRAC Manuals stored in the laboratory NSF Earth X ray Analysis Center EXACt in the vertical file After training the Procedure User should refer to the manuals when questions arise or consult with the Machine Custodian to solve specific problems 8 5 Sample Control Sample identification will be based on the unique identifier labeled on the sample This will typically be an etched identification on the plate holder for analysis 8 6 Performing the Standard Operation Procedure for XRD Siemens Diffraktometer D5000 Qualitative Scanning 8 6 1 8 6 2
18. ine solids based on these properties for mineral composition of the samples The construction of the analytical chamber allows samples of various sizes to be analyzed The D 5000 is completely computer controlled for data acquisition Phase identification may also be automated by search match software and a CD ROM archive of the JCPD tables 8 2 Sample Preparation samples to be examined with the XRD machine must be in a form or size that can be inserted into or attached to and XRD D 5000 stage mount and very well compacted Quantitative microanalysis routines assume that all samples for analysis will be relatively flat and that analysis sites will be normal to the beam incidence Sample requirements for powder XRD vary with the nature of the material A typical sample holder is a 2 mm thick plate with a 20 mm square hole in the center For materials that diffract strongly many inorganic materials Scotch double tape is placed over the hole with the sticky side up About 10 20 mg of the material of interest is then spread on the tape and smoothed flat The tape is primarily amorphous and so does not generally interfere with the pattern being collected 11 For materials that diffract less strongly such as organic molecular crystals more sample 100 200 mg must be used One way of doing this is to tape or glue a microscope slide to the back side of the sample holder The depression in the holder is then filled with sample and smoothed
19. ith the Machine Custodian Safety Considerations Normal operating conditions as performed by trained Procedure Users present no safety hazards Environmental Conditions Normal interior building temperature and humidity are acceptable for the operation of the XRD D5000 oystem Cooling water for the XRD D5000 diffusion pump and electronics chassis is supplied by the building chilled water system maintained in the range of 55 to 65 degrees Fahrenheit Ambient air temperature for the XRD D5000 System should range between 60 and 80 degrees Fahrenheit Note f environmental conditions move out of range during operating the XRD D5000 system in WDS mode Procedure Users should take extra precaution to ensure system stability by checking standards often Calibration of Magnification The Machine Custodian or delegated individual will check the accuracy of the computer generated micrometer marker annually against NIST Standard Reference Material Catalog SEM magnification Standard Tolerance is 10 If out of tolerance it will be the Machine Custodian s responsibility to arrange for repair of the instrument so that it will be within tolerance 33 9 0 RECORDS The Procedure User is responsible for submitting the following records to the Machine Custodian Lab Instrumentation specialist to be storage at the UPR NSF Earth X ray Analysis Center EXACt F 304 C 9 1 Log Book or Notebook records of the sample handling and results of analy
20. l measures atomic spacings in crystals using diffraction of approximately monochromatic x radiation It can be used to characterize solid samples ranging in size This SOP states the responsibilities and describes the methods procedures and documentation used to obtain X ray powder diffraction data from Siemens D5000 X ray Powder Diffractometer at the UPR NSF Earth X ray Analysis Center EXACt Geochemistry Facilities Department of Geology UPR Mayag ez Campus 2 0 SCOPE This SOP is a mandatory document and shall be implemented by all Researcher Faculty member Technician and or students participants when using the XRD Diffraktometer D 5000 for the collection of XRD data This SOP covers elementary physical operation of the instrument and radiation safety compliance requirements Data interpretation is beyond the scope of this manual 3 0 TRAINING 3 1 A All users of this SOP will be trained by reading the procedure and the training is documented in accordance with the GLP s 3 2 The Geology Task Leader will monitor the proper implementation of this procedure and ensure that relevant team members have completed all applicable training assignments in accordance with GLP s 4 0 DEFINITIONS 4 1 Alignment The orientation of sample beam and detector axes Ideally all three coincide with the eucentric point 4 2 Circle Any of the separate mechanisms which rotate the sample or detector under the x ray beam Circle 1 rotates the sa
21. lemental information may be processed following instructions in the XRD D5000 and Diffrac Plus Software Manuals Image and elemental information may be photographed and or printed on paper following instructions in the reference Manual if an electronic copy or a hard copy is desired The software package Diffrac Plus comprises software used for acquisition and reduction of quantitative elemental data 8 7 1 Find the DIFFDAT1 Folder in the Local Disk C 1 objext s selected E My Computer Pistort 48a O ai efra Peer Ej Ratus sees Hysa Beva roca aloa 42 gg zs 25 8 7 2 Open it and find the file with the given name in the 7 5 16 8 7 3 Click over the Diffrac Plus icon to open the software and then click the EVA to open the Storage Data software Se Diffrac Plus 1 File Edit View Favorites Tools Help My D 4m Back gt b Search L4 Folders cS As UI X A Ez Address EJ Diffrac Plus 1 E Config DIFFRAC PLLIS DQuant EditDQL Environment Eva Immediate JOB Ma D iffr ac P l us 1 Evaluation Measurement Measurement Immediate Measurement 5 5 Shortcut vice PDFMaint Service Status Display Uninstall Location C DiffPlus Contact Diffrac Plus R Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal EP pce Diff Fa n Offi Wi Location C DiffPlus 448 bytes te My Computer A Astart e B x w all
22. mal Arial Ari Er zn Z Sample position E All Entries 7 cle sec 5 Diy Sit Anti Sli Aug 1 Buy 2 Aux 3 Aum d TITTLE TTT Adel T Aux standard Det Sit i Rotation NO zj Shutter Eon rum E Start anl E Stop dw Sees 0 u STOP 43 m Scantyoe zz Festart Data Collection x Measure Measure gt For Help press F1 o6 16 06 10 35 37 E Select and click on Diffractomaeter al Ble ER Draws Le AutoShapes A w LIO EJ i gl ig w A S25 Page 10 Sec 1 0010 ak 1 3 in Col REC TRE EXT OWR Engish Uus X Pstart Bs pw amp computational amp e CisoP s i sOP Semens tRD Cypiffrac Plus 1 4 biffractometer aS 10 35 am 24 8 6 24 Select Init All Drives The goniometer will reach the vertical position 8 6 25 Back on the left side of the panel in front of the XRD machine e Decrease the current mA and the voltage kV 10 units by 10 units waiting 1 minute between each time to get the minimum values of 5 mA and 20 kV Press the vellow button Press the red button Then an X ray indicator will turn off Turn the key Turn on the green switch of ON and OFF 8 6 26 The Chiller must turn off 30 minutes after operating the XRD machine at pressure of 60 80 psi and a temperature of 65 F 8 7 Data Acquisition and Reduction Data may consist of image information and or elemental information Image and e
23. mple about a vertical axis Circle 2 turns the detector also about a vertical axis Circle 3 tilts the sample about a horizontal axis and designated chi Circle 4 rotates the sample about an axis normal to the sample surface through the center of the holder and called phi c 4 3 4 4 4 5 4 6 4 1 4 8 Note Circles 1 and 2 are independent Circle 3 is mounted on top of circle 1 and circle 4 is mounted on top of circle 3 Counts A measure of signal intensity For a given sample the apparent signal intensity will depend on the scanning parameters with small step sizes giving higher numbers D5000 D5000 is the model name of the XRD manufactured by oiemens Incorporated purchase date month year serial number Eucentric The point at which all four goniometer axes intersect in space In the ideal case the sample surface coincides with the eucentric as does the point illuminated by the xray source and the point observed by the detector GLP s Good Laboratories Practices Goniometer The mechanism which supports the sample and detector allowing precise movement Machine Custodian The Machine Custodian is responsible for Siemens Diffraktometer D5000 maintenance and User instruction This includes calibration basic repairs and software data taken and electronically stored system backups and all instruction and training of Procedure Users 4 9 4 10 4 12 4 13 4 14 Monochromet
24. n C DiffPlus i Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal Location C DiFFPlus 448 bytes te My Computer Astar 2 B x w E amp Computational Geo CySOP s il soP siemens xRD SyDiffrac Plus 1 Diffractometer 1 a CS SBS 10 31 am 22 8 6 22 Once the sample was analyzed Return the goniometer to the original position vertical by clicking the Immediate Measurements to run the XRD amp Diffrac Plus 1 My File Edit View Favorites Tools Help Beck 9 Ga Qsearch Gyrokers Us Os X A EA Address y Diffrac Plus 1 m H eiii P Config DIFFRAC PLLIS DQuant EditDQL Environment Eva Immediate JOB Maintenance Diffrac Plus 1 Evaluation Measurement Measurement gt is E Immediate Measurement XS Md Shortcut vice ay PDFMaint Service Status Display Uninstall Location C DiffPlus Contact Diffrac Plus Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal Location C DiffPlus 448 bytes g My Computer A if start 4 az w E amp Computational Geo SOP s amp oP siemens xRD ypiffrac Plus 1 diffractometer 1 i tS SEIS 10 31 am 23 8 6 23 Select and click on Diffractometer option M SOP Siemens XRD Di viffractometer 1 Adjust i 0 x le x File Edt View Inse F V a pie Help e a question For help X DEURA ANLA Ay in elele 2 vj 44 Nor
25. n a tray at the bottom Samples can be run wet or dry A cover is placed on the bowl and then the bowl is mounted in the machine In the picture below one bowl has been fastened down and the other has not yet been secured Once the bowls are mounted and secured the cover is lowered and the machine can be operated 13 Each bowl sits on an independent rotatable platform and the entire assembly of four bowls is also rotated in a direction opposite to the direction of the bowl platform rotation This action is a lot like the teacup and saucer rides commonly found in amusement parks In planetary action centrifugal forces alternately add and subtract The grinding balls roll halfway around the bowls and then are thrown across the bowls impacting on the opposite walls at high speed Grinding is further intensified by interaction of the balls and sample Planetary action gives up to 20 g acceleration and reduces the grinding time to about 2 3 of a simple centrifugal mill one that simply spins around Grinding media are available in agate sintered corundum tungsten carbide tempered chrome steel stainless steel zirconium oxide and polyamide plastic The exact type of bowl and balls that are used depend on the type of material being ground For example very hard samples might require tungsten carbide balls in steel bowls For typical use agate is a good choice As with any method of grinding cross contamination of the sample with t
26. o 50 mA for the current and 45 kV to 55 kV and for the voltage to increase the intensity of the peaks 8 6 6 2 An important rule of thumb e When turning a tube up increase the kV first and then increase the mA e When turning a tube down decrease the mA first and then decrease the kV 8 6 7 Now open the XRD clear door to access the goniometer 8 6 8 Remove the knob to access the goniometer and place the sample s in order from 1 to 40 positions 8 6 9 Choose between 1 mm and 2 mm slit Note Usually for geological samples use 2 mm and for thin films 1 mm 8 6 10 Now on the desktop of the computer click over the Diffrac Plus icon to open the software 8 E 11 Click the immediate reme to run the XRD for a fast run and to find or have an idea of the relatively of unknown peaks of the sample to be analyzed f no skip this step and go directly to step 8 6 14 to run the measurements 16 m mm Config DIFFRAC PLUS DQuant EditDQL Environment Eva Immediate JOB Maintenance Evaluation Measurement Measurement Diffrac Plus 1 gt i Ee Immediate Measurement XS Md Shortcut vice ler PDFMaint Service Status Display Uninstall Location C DiffPlus Contact Diffrac Plus Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal Location C DiffPlus l4 48 bytes e My Computer P if start 2 a3 x wj amp Computational Geo ysor s W 50P Siemens XRD ipitfrae Pl
27. oP Cameca s il SOP Siemens x w SOP Siemens x DIFFRAC PLUS fic XCH 3 Guan d OE ED 10 49am 8 7 14 XCH displays the Save As dialog box e Browse to the folder in which you want to create the new file e Enter its name in the File name field e Then click Save 3l 8 7 15 Click on Eva icon to see your graph once again This will save your graph as EVA extension amp V Diffrac Plus 1 File Edit View Favorites Tools Help Back 4 seach Fyrolders C ME GE Xx A Ea Address y Diffrac Plus 1 mw Config DIFFRAC PLLIS DOuant EditDQL Environs i JOB Maintenance Diffrac Plus 1 Evaluation EZ urement Measurement a gt a p Immediate Measurement XS Md Shortcut vice ter PDFMaint Service Status Display Uninsta Location C DiffPlus Contact Diffrac Plus 2 Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal ocation C DiFFPlus 448 bytes My Computer a Astart 4 B x v all amp Computational Geo CXSOP s i oP siemens xRD Sypiffrac Plus 1 Diffractometer 1 SSA 10 31 am 8 7 16 This graph only can be opened at EVA software This will save your graph analyzed with the Search Match option as follow in the figures CWA Calta Fie ft ew Wires Help bie pos a maa fz Imc aa aL tel o eo Al Ll em Li Y Damia 3n NEM CFA a E Fw ia 2 Ra 1 EZES E Fei j rammCu Pater WEN 7702243 Fiore ICaF ZI
28. of crystals i e a powdered sample show that the diffracted beams form continuous cones 7 0 e A circle of film is used to record the diffraction pattern as shown e Each cone intersects the film giving diffraction lines The lines are seen as arcs on the film e For every set of crystal planes by chance one or more crystals will be in the correct orientation to give the correct Bragg angle to satisfy Bragg s equation Every crystal plane is thus capable of diffraction Each diffraction line is made up of a large number of small spots each from a separate crystal Each spot is so small as to give the appearance of a continuous line If the crystal is not ground finely enough the diffraction lines appear speckled EQUIPMENT Descriptions of equipment constituting the XRD Diffraktometer D5000 system are provided below 7 1 XRD Siemens Diffraktometer D5000 The Siemens D5000 instrument has a large diameter goniometer 600 mm low divergence collimator and Soller slits Attachments include sample spinner stages reflection transmission holders incident or diffracted beam monochromators zero background holders and odd sample shape holders The instrument is useful for both powder and bulk materials This diffractometer is the best utilized for high precision work Data collection is performing under computer control using the Diffrac Plus software application 10 8 0 PROCEDURE Note All personnel performing work un
29. rac Plus 1 Evaluation Measurement Measurement s f Immediate Measurement XS Ma Shortcut vice er PDFMaint Service Status Display Uninstall Location C DiffPlus Contact Diffrac Plus R Modified 05 09 05 3 50 PM Size 448 bytes Attributes normal zt pce Diff Fa h Offi Wi Location C DiffPlus 448 bytes te My Computer p if istart az al Computational Geo ysor s W SOP Siemens XRD upiffrac Plus amp i1 4Diffractometer 1 A CS SES 10 31 am 18 8 6 16 Select and click on Measurement Set Up option and then click on Qualitative Simple to edit and set up the parameters such as e Comment Starting Angle Stopping Angle otep Size Time Step Afa pracu 13 File Edit view Favorites Tools Help E 4m Back b A Search L 4 Folders J x n X A Ez A adres oraes o o E Contig DIFFRAC PLUS DQuant EditDOL Environment Eva Immediate JOB Maintenance Diffrac Plus f T ENS Bi x ement setup EditDQL Shortcut Location C DiffPlus EC dit Qualitativ easurement Instructions x Modified 05 09 05 3 5C Edi Size 452 bytes Comment Eram E nC User Task File Browse Attributes normal Default Scan Parameters for a Locked Coupled Scan 2Theta Start 10 0000 deg Stop 30 0000 deg Step size 0 0200 deg Time Step 1 00000 Delay time 0 00000 Steps 4001 Scan time 01 06 41 00 Slits amp Rot Cancel Range Entries gt
30. sis relevant to Production of XRD data 9 2 Data submittals will be storage in the electronic database 9 3 It is obligation of the user to backup the data obtained 9 4 Data will be held by the laboratory for thirty 30 days after which it may be eliminated from departmental files 10 0 REFERENCES The following documents have been cited within this procedure by e Siemens D5000 X ray Diffractometer Manual Siemens Analytical X Ray Instruments Inc 6300 Enterprise Lane Madison WI 53719 e Siemens D5000 X ray Diffractometer Operation and Maintenance Training Course Siemens Analytical X Ray Instruments Inc 6300 Enterprise Lane Madison WI 53719 Bruker Advanced X Ray Solutions DIFFFRACP User s Manual http www bruker axs de http erproject lanl gov docs Quality SOP SOP 09 02R1T pdf http geology uprm edu facilities exact html http geology uprm edu facilities labrules exact doc http www ilpi com inorganic glassware xrd html http www ilpi com inorganic glassware mortarpestle html http www ilpi com inorganic glassware ballmill html 34
31. t Company Site Dept of Geology No RAW File Pos Sample Identification Parameter File Usertask File Mode Status T S Modified 0E Location C e b Size 452 by Attributes co NN AUN E e 4 Y Delete Copy Paste Insert Skip Reset Recover Browse Mode Default directory C ADIFFDAT 1S Sample RAW File DQL File UTF File NO ACTIVE JOB Active RAW File For Help press F1 NUM pa Location C DiffPlus 452 bytes g My Computer P PAstart S m x jw E computati Casos sop siem Cubiffrac Plu Sunnen FaeUNTITLED Suntituep HARG 11 34 am 2 8 6 20 In this previous window fill the table writing down the e No gt for Sample order number Raw file gt for Sample name Pos for Sample number position Parameter File gt write the name of file created on DQL Etc Save as Then click on Execute Job to run the XRD machine 8 6 21 Back on the Diffrac Plus window click the Status Display to follow the performing of the XRD machine Diffrac Plus 1 File Edit View Favorites Tools Help gt Gsearch Gyrolders C HS GE X A Ea Address y Diffrac Plus 1 n Config DIFFRAC PLUS DQuant Environment Eva Imm e JOB Main Diffrac Plus 1 Evaluation Measurement Measurement ET MIC PDFMaint Service Status Display uni Il Contact Diffrac Plus Immediate Measurement JJ XS Shortcut e Locatio
32. us 1 Diffractometer 1 f 4 lt a HS 10 31 am 8 6 12 Select and click on Diffractometer option M sor siemens ZRD Dilli piffractometer Adjust 18 x File Edit View Inse w Help a question for help X iD us d 3 gic Nas ut alale o x Al vivi M Normal Arial Ari E MEE m zum Sample position B All Entries n E ctual Div Slit Anti Slit mmm amp Vdd E Aux Standard Det Siit In i Rotation GN oFF Shutter Open Aco xj Start z j zw Banned zi i STOP TL E uc Scantype Restart Data Collection lt lt Measure Measure gt gt For Help press F1 mn 06 16 06 10 35 37 A Select and click on Diffractometer n G EJ 4 Draw Lg AutoShapes w CLIO amp 3 4l Sli O w A S Page 10 Sec 1 10 10 At 1 3 In 3 coll REC TRK EXT OYR English L S PAstart GB x jw E computational Geo CusoP s soP siemens xRD Cypiffrac Plus t Diffractometer HARM 10 35 am 17 8 6 13 Select Init All Drives Note Check the Door is closed 8 6 14 In this option set up the parameters 8 6 15 Back on Diffrac Plus window click the Edit DQL L Diffrac Plus 1 ww File Edit View Favorites Tools Help Back 3g search Gyrolders C Um GZ X A Ea Address E Diffrac Plus 1 mE il I t Config DIFFRAC PLUS DQuant EditDOL Environment Eva Immediate JOB Maintenance Diff
Download Pdf Manuals
Related Search