ARL 9900 INTELLIPOWER Series User Manual AA83654 USER MANUAL ARL 9900 INTELLIPOWER SERIES Report MANUAL AA83654-02 No Language E Date August 2007 Department Doc Author RSc AA83654-02 The information in this document is subject to change without notice. We assume no responsibility for any errors that may appear in this document. Die Angaben in diesem Dokument können ohne vorherige Information geändert werden. Wir übernehmen keine Verantwortung für eventuelle Mängel in diesem Dokument. Les informations contenues dans ce document sont sujettes à changement sans préavis. Nous n’assumons aucune responsabilité pour toutes erreurs éventuelles contenues dans ce document. Ci riserviamo il diritto di modificare le informazioni contenute nel presente manuale senza preavviso e non ne assumiamo nessuna responsabilità quanto ad eventuali errori che potrebbero esservi accidentalmente introdotti. Las informaciones contenidas en este documento pueden ser modificadas sin previo aviso. Nosotros declinamos toda responsabilidad sobre eventuales errores contenidos en este documento. los AA83654-02 PAGE DE MODIFICATION ÄNDERUNGSANGABEN REVISION CONTROL SHEET Date Datum Date 2005 August 2007 August October Modification Description Änderung Beschreibung Revision Description 00 Creation of manual 01 02 Introduction of INTELLIPOWER NEXRD General updating AA83654-02 TABLE OF CONTENTS Table of Contents 1 INTRODUCTION..................................................................................... 1-1 THE ARL 9900 SERIES ...........................................................................................1-1 Front View of the Instrument with the 12 Position Sample Changer ....................1-1 Front View of the Instrument with the X-Y Sample Changer ................................1-2 Front View of the Instrument with Single position Manual loading .......................1-2 View of the Instrument with the X-Y Sample Changer OEM version....................1-3 View of the Instrument integrated for Automation System ARL SMS 900............1-3 X-RAY FLUORESCENCE SPECTROMETER PRINCIPLE .....................................1-4 2 SAFETY.................................................................................................. 2-1 GENERAL WARNINGS............................................................................................2-1 SAFETY DEVICES AND CIRCUITRY......................................................................2-2 Emergency stop push button................................................................................2-3 Restart push button..............................................................................................2-3 X-ray ON lamp .....................................................................................................2-3 Buzzer ..................................................................................................................2-4 Interlock safety systems .......................................................................................2-4 3 INSTRUMENT DESCRIPTION ............................................................... 3-1 THE ARL 9900 INTELLIPOWER SERIES INSTRUMENT CONFIGURATIONS......3-1 VIEWS OF THE ARL 9900 INTELLIPOWER SERIES INSTRUMENT.....................3-2 Front view with 12 Position Sample Changer.......................................................3-2 Front View with the X-Y Sample Changer............................................................3-3 Back View of the Instrument.................................................................................3-4 INSTRUMENT DISPLAY..........................................................................................3-6 Spectrometer Status Display................................................................................3-6 X-ray Tube Status Display....................................................................................3-7 Goniometer Status Display...................................................................................3-7 XRD goniometer Status Display...........................................................................3-7 INSIDE THE ARL 9900 INTELLIPOWER SERIES INSTRUMENT ..........................3-8 INSTRUMENT VIEW................................................................................................3-8 Electronic Rack ..................................................................................................3-11 ANALYTICAL CONDITIONS ..................................................................................3-13 I AA83654 ARL 9900 INTELLIPOWER Series User Manual Table of Contents Goniometer ........................................................................................................3-13 The Universal F45 Goniometer ......................................................................3-13 Configuration table.........................................................................................3-14 The SmartGonio™ .........................................................................................3-15 Configuration table.........................................................................................3-15 Compact XRD diffractometer .............................................................................3-16 Unique integrated phase analysis ..................................................................3-16 FULL XRD DIFFRACTOMETER ............................................................................3-17 Primary Beam Filter (Option)..............................................................................3-19 List of Primary Beam Filters (Option) .............................................................3-19 FIXED CHANNELS ................................................................................................3-20 Configuration of the monochromators............................................................3-20 ANALYSIS ENVIRONMENT ..................................................................................3-22 Environment Setting...........................................................................................3-22 Gas Regulation (Optional)..................................................................................3-22 Thermal Regulation............................................................................................3-22 SAMPLE EXCITATION ..........................................................................................3-23 X-ray Tube .........................................................................................................3-23 X-ray Power Supply ...........................................................................................3-23 Ecological Mode.................................................................................................3-24 X-ray Tube Safety Interlock................................................................................3-25 X-ray Tube Cooling System for ARL 9900 INTELLIPOWER Series 3600W and 4200W.........................................................................................................3-25 X-ray Tube Cooling System for ARL 9900 INTELLIPOWER Series 1200W 2500W................................................................................................................3-25 SAMPLE HANDLING SYSTEMS ...........................................................................3-26 Manual sample loading ..................................................................................3-26 Sample loading with 12 position sample changer ..........................................3-27 Large X-Y sample changer ............................................................................3-28 Transport belt(s) and docking port .................................................................3-30 Suction option ................................................................................................3-31 Automation.....................................................................................................3-32 Automatic samples.........................................................................................3-32 Manual samples, Setting-up, Control and Type standard samples (SCT) .....3-32 OXSAS / OEM software option ......................................................................3-33 SAMPLE HOLDERS ..............................................................................................3-34 Cassettes ...........................................................................................................3-34 Centring rings.....................................................................................................3-35 Sample supports ................................................................................................3-36 II ARL 9900 INTELLIPOWER Series User Manual AA83654 Table of Contents SAMPLE LOADING SYSTEM ................................................................................3-37 Sample Loading Process ...................................................................................3-38 4 INSTRUMENT PREPARATION.............................................................. 4-1 SWITCH ON THE INSTRUMENT ............................................................................4-1 With 12 positions cassette magazine ...................................................................4-2 With X-Y magazine ..............................................................................................4-3 SWITCH ON THE PC...............................................................................................4-4 START UP PROCEDURE WITH OXSAS SOFTWARE. ..........................................4-4 Instrument Configuration and Initialisation ...........................................................4-5 Instrument Initialisation ....................................................................................4-5 Perform a goniometer initialisation as described below. ..................................4-6 Gas Supply ......................................................................................................4-6 Environment Setting.........................................................................................4-8 Switch on the XRF X-ray Tube Power Supply................................................4-10 Switch on the Full XRD X-ray Tube Power Supply (applicable on Workstation only) ...........................................................................................4-11 Eco Mode Setting...........................................................................................4-12 INSTRUMENT TECHNICAL DATA ........................................................................4-14 5 SAMPLE PREPARATION ...................................................................... 5-1 Sample Preparation for Solids..............................................................................5-2 Sample Preparation for Powders .........................................................................5-4 Briquet method.................................................................................................5-4 Fusion technique..............................................................................................5-5 Sample Preparation for Liquids ............................................................................5-5 Work-up techniques .........................................................................................5-5 6 ROUTINE ANALYSIS............................................................................. 6-1 CONCENTRATION ANALYSIS WITH OXSAS ........................................................6-1 Performing a Quantitative Analysis in manual mode............................................6-1 With 12 position magazine ...............................................................................6-1 With X-Y magazine cassette version ...............................................................6-2 With X-Y magazine sample version .................................................................6-3 INTENSITY MEASUREMENT WITH OXSAS ..........................................................6-7 QUALITATIVE ANALYSIS WITH SMARTGONIOTM OR UNIVERSAL GONIOMETER AND OXSAS .................................................................................6-10 With 12 position magazine .............................................................................6-10 With X-Y magazine cassette version .............................................................6-11 With X-Y magazine sample version ...............................................................6-12 III AA83654 ARL 9900 INTELLIPOWER Series User Manual Table of Contents QUALITATIVE ANALYSIS WITH COMPACT XRDTM AND OXSAS.......................6-21 With 12 position magazine .............................................................................6-21 With X-Y magazine cassette version .............................................................6-22 With X-Y magazine sample version ...............................................................6-23 Investigating Diffractograms...............................................................................6-28 QUANTITATIVE PHASE ANALYSIS WITH COMPACT XRD CHANNEL ..............6-30 QUALITATIVE ANALYSIS WITH FULL XRDTM AND OXSAS ................................6-30 With 12 position magazine .............................................................................6-30 With X-Y magazine cassette version .............................................................6-31 With X-Y magazine sample version ...............................................................6-32 Investigating Diffractograms...............................................................................6-37 QUANTITATIVE PHASE ANALYSIS WITH FULL XRD CHANNEL .......................6-38 With 12 position magazine .............................................................................6-38 With X-Y magazine cassette version .............................................................6-39 With X-Y magazine sample version ...............................................................6-40 Running Visual Crystal.......................................................................................6-42 7 ANALYTICAL ASSISTANT FOR OXSAS .............................................. 7-1 Launching the Online Help ...................................................................................7-1 Using the Online Help ..........................................................................................7-2 Navigating the Help session.................................................................................7-2 Printing Help topics ..............................................................................................7-3 About the Analytical Assistant ..............................................................................7-3 To open the Analytical Assistant ..........................................................................7-4 CREATING A METHOD I: BASICS..........................................................................7-5 Defining a Method name ......................................................................................7-5 Defining Concentration ranges.............................................................................7-5 Selecting Elements ..............................................................................................7-6 Adding Elements ..................................................................................................7-6 Setting Sample Preparation parameters ..............................................................7-8 Scan/Energy Profiles............................................................................................7-9 Saving a Method ................................................................................................7-11 Running a Batch.................................................................................................7-12 8 INSTRUMENT CALIBRATION ............................................................... 8-1 INTRODUCTION......................................................................................................8-1 INSTRUMENT CALIBRATION WITH OXSAS..........................................................8-1 IV ARL 9900 INTELLIPOWER Series User Manual AA83654 Table of Contents 9 PERIODIC MAINTENANCE ................................................................... 9-1 SOFTWARE DATA SECURITY ...............................................................................9-1 To backup the database.......................................................................................9-2 To restore a database ..........................................................................................9-5 INSTRUMENT HARDWARE ....................................................................................9-7 Sample cassettes.................................................................................................9-7 12 Position Sample Magazine..............................................................................9-7 X-Y magazine trays..............................................................................................9-7 Vane stage pump oil level ....................................................................................9-7 Deionized water level .........................................................................................9-11 Dust filter............................................................................................................9-12 AR-CH4 P10 GAS...................................................................................................9-14 ANALYTICAL PARAMETERS................................................................................9-15 Monochromators ................................................................................................9-15 Energy profiles and detectors resolutions ......................................................9-15 WDS Goniometer ...............................................................................................9-19 Investigate energy profile and detector resolution..........................................9-19 Compact XRD Goniometer.................................................................................9-23 Investigate energy profile and detector resolution..........................................9-23 Full XRD Goniometer for Workstation ................................................................9-25 Investigate energy profile and detector resolution..........................................9-25 Investigate Goniometer scans............................................................................9-27 Principle of Goniometer Positioning ...............................................................9-27 About Position Calibration..............................................................................9-27 Tables of Crystals, Detectors and Collimators combinations .........................9-28 Goniometer F45 Position Calibration Specifications ......................................9-28 Smart GonioTM Position Calibration Specifications.........................................9-30 Compact XRD Position Calibration Specifications .........................................9-31 Full XRD for Workstation Position Calibration Specifications.........................9-32 To perform a scan with WDS goniometer ..........................................................9-33 To perform a scan with Compact XRD goniometer ............................................9-35 To perform a scan with Full XRD goniometer.....................................................9-37 ARL 9900 SERIES INSTRUMENT GLOBAL MAINTENANCE...............................9-39 A APPENDIX A ..........................................................................................A-1 INTRODUCTION..................................................................................................... A-1 X-RAY EMISSION................................................................................................... A-1 AA83654 ARL 9900 INTELLIPOWER Series User Manual V Table of Contents Photoelectric absorption...................................................................................... A-2 Scattering............................................................................................................ A-4 Transmission....................................................................................................... A-5 NOMENCLATURE USED IN XRF........................................................................... A-6 INSTRUMENTATION.............................................................................................. A-7 X-ray Tube .......................................................................................................... A-7 Continuum....................................................................................................... A-8 Characteristic spectra and choice of the X-ray tube target ............................. A-8 Spectral Line Interference ............................................................................... A-9 Window thickness ........................................................................................... A-9 DISPERSION ........................................................................................................ A-10 Sequential Instruments ..................................................................................... A-10 Simultaneous Instruments................................................................................. A-11 Instrument Components .................................................................................... A-12 Goniometer ................................................................................................... A-12 Collimators .................................................................................................... A-13 Crystals ............................................................................................................. A-14 Diffraction...................................................................................................... A-14 Multilayer Structures ..................................................................................... A-15 Reflectivity and Resolution............................................................................ A-15 Dispersion Power.......................................................................................... A-16 Stability ......................................................................................................... A-17 Higher orders of diffraction............................................................................ A-17 Resume............................................................................................................. A-18 DETECTION.......................................................................................................... A-19 Gas filled counters ............................................................................................ A-19 Primary Ionization ......................................................................................... A-20 Avalanche ..................................................................................................... A-20 Characteristics .............................................................................................. A-22 Scintillation Counters ........................................................................................ A-23 Pulse Height Discriminator (PHD) ..................................................................... A-24 Final output ....................................................................................................... A-25 VI ARL 9900 INTELLIPOWER Series User Manual AA83654 1 INTRODUCTION INTRODUCTION Chapter 1 1 INTRODUCTION The ARL 9900 Series X-ray fluorescence allows measurement of up to 84 elements of the periodic table in samples of various forms and nature: solids or liquids, conductive or non-conductive. Typical samples include glasses, plastics, oils, all metals, ores, refractory, cement and geological materials. All samples must not react with the X-rays. The solid samples must support the analysis under vacuum and the liquid samples are analysed under helium environment. Advantages of XRF over other techniques are speed of analysis, generally easy sample preparation, very good stability and precision and wide dynamic range. The ARL 9900 Series provides high performance measurements on all types of samples. The heart of the ARL 9900 can be made of various modules: monochromators for rapid, dedicated routine analysis, a Moiré fringe Universal or SmartTM goniometer for flexible elemental analysis and an integrated X-ray diffraction system providing a wide range for phase and mineral analysis. The combination of fixed channels and goniometer guarantees speed, flexibility and reliability of analysis. Four versions are available. ♦ ARL 9900 OASIS is the low power version, with a 1.2 kW generator, without external water cooling. ♦ ARL 9900 INTELLIPOWER is the mid power version, with a 2.5 kW generator, without external water cooling. ♦ ARL 9900 XP is the standard version, with a 3.6 kW generator. ♦ ARL 9900 XP+ is the high performance version, with a 4.2 kW generator. Front View of the Instrument with the 12 Position Sample Changer Figure 1.1 AA83654 ARL 9900 INTELLIPOWER Series User Manual 1-1 Chapter 1 INTRODUCTION Front View of the Instrument with the X-Y Sample Changer Figure 1.2 Front View of the Instrument with Single position Manual loading Figure 1.3 1-2 ARL 9900 INTELLIPOWER Series User Manual AA83654 INTRODUCTION Chapter 1 View of the Instrument with the X-Y Sample Changer OEM version Figure 1.4 View of the Instrument integrated for Automation System ARL SMS 900 Figure 1.5 AA83654 ARL 9900 INTELLIPOWER Series User Manual 1-3 Chapter 1 INTRODUCTION X-ray Fluorescence Spectrometer Principle The sample to be measured is loaded into the spectrometer and excited by the X-ray beam coming from the X-ray tube: An Incoming x-ray photon strikes an electron, the electron breaks free and leaves the atom.This leaves a void (see next figure). Figure 1.6 This void is filled by an electron from a higher energy. The electron releases energy (fluoresces) as it drops in the form of an x-ray photon. x-ray photon Figure 1.7 The spectrum of the tube is composed of the characteristic wavelengths of the anode elements and the continuum. The emitted radiation from the sample is composed of the tube spectrum and the characteristic wavelengths of the elements in the sample. The reflected beam is guided onto a dispersive system called, in our case, goniometer. This goniometer produces spectra of lines which are in relation with the elements included in the measured sample. The XRD system collects in its detector the diffracted X-ray of one specific wavelength emitted by the X-ray tube. The incident beam is diffracted by the various crystallographic planes of the crystallites which are present in the sample. For more details about XRD analysis, please refer to the specific brochure about the “ARL 9900 - Integrated XRD system”. 1-4 ARL 9900 INTELLIPOWER Series User Manual AA83654 INTRODUCTION Chapter 1 Figure 1.8 All XRF and XRD spectrometers measure intensities. The concentrations are obtained only once the instrument has been calibrated. It should be stressed that an XRF quantometer is a very accurate comparator, but the accuracy of the final analysis is entirely dependent on the quality of the standard samples used for calibration. The intensity concentration relationship is generally linear, but in some cases the curve can be second degree. C(%) = a0 + a1 * I C(%) = a0 + a1 * i + a2 * I2 First degree Second degree Where: i is the intensity measured by the XRF spectrometer aj are the constants computed during the calibration C is the concentration in % In practice, the intensity of an element is not only a function of the concentration of the element analysed but may also be influenced by interferences such as line overlapping, absorption or enhancement due to constituents of the matrix. The Chapter Analysis Principle gives more information. AA83654 ARL 9900 INTELLIPOWER Series User Manual 1-5 2 SAFETY SAFETY Chapter 2 2 SAFETY General Warnings The XRF instrument uses several components, which can be dangerous to manipulate. The signs shown below are stuck to covers and panels etc. to warn you: Risk of electrocution Switch off the power before removing this panel or part. Figure 2.1 Poisonous Avoid any contact with these components and their support (for example: Beryllium window or TLAP crystal). Wear gloves when manipulating these components. Figure 2.2 X-rays This icon indicates a panel or a part of X-ray shielding. Switch off the X-ray tube power supply before removing this panel or part. Figure 2.3 As a general rule the user must contact the nearest local service if he needs to open the instrument. In case of problem or injury, we will take no responsibility if the user has removed one or several cover or panels fitted with one of the signs shown above. AA83654 ARL 9900 INTELLIPOWER Series User Manual 2-1 Chapter 2 SAFETY Safety devices and circuitry X-Ray On Lamps Restart Button Emergency Stop Button Figure 2.4 - Instrument with 12 position Magazine X-Ray On Lamps Restart Button Emergency Stop Button Figure 2.5 - Instrument with X-Y Sample changer 2-2 ARL 9900 INTELLIPOWER Series User Manual AA83654 SAFETY Chapter 2 X-Ray On Lamps Emergency Stop Button Figure 2.6 - Instrument with Manual Loading System or Automation System Emergency stop push button The emergency stop push button is located on the right front side of the instrument. In case of emergency the red push button is available to shut down the overall electrical power supply of the instrument. The instrument power distribution is protected by a class 4 safety circuit, matching the TUV PTB safety prescriptions. When pressing the emergency stop push button, both the power of the spectrometer and the Xray tube power supply are switched off. Important: The computer accessory plug remains live! Restart push button The Restart button is located close to the Emergency Stop Button. It allows power-up the instrument. Pressing the restart push button, the instrument power-up is possible only if: ♦ the emergency stop button is released ♦ the class 4 safety circuit redundancy is fulfilled ♦ the safety circuit power components do not show any defect X-ray ON lamp The “X-ray ON” lamps are controlled by the X-ray tube power supply. The lamps are on whenever the X-ray power supply is on. Two bulbs are situated under the cover. If both bulbs are broken the X-ray tube power supply switches off or cannot be switched on. It is important to use specific bulbs; otherwise there is risk of destroying some electronic parts of the instrument! AA83654 ARL 9900 INTELLIPOWER Series User Manual 2-3 Chapter 2 SAFETY Buzzer When the X-ray tube power supply is switching on, an internal buzzer is activated for few seconds. Interlock safety systems Each component preventing X-ray leaks is secured by a safety switch and is connected to the X-ray tube power supply interlock. All these contacts must be closed to switch on the X-ray power supply. As soon as one part is removed or missing the X-ray power supply switches off immediately. THE SAFETY CIRCUITS MUST NEVER BE BY-PASSED. 2-4 ARL 9900 INTELLIPOWER Series User Manual AA83654 3 INSTRUMENT DESCRIPTION INSTRUMENT DESCRIPTION Chapter 3 3 INSTRUMENT DESCRIPTION The ARL 9900 INTELLIPOWER Series instrument requires about 1.5 square meter floor space and is therefore designed to be placed in reduced space areas. The ARL 9900 INTELLIPOWER Series instrument configurations 3 sample loading systems are available: 12 Positions sample magazine X-Y sample manipulator Single cassette or sample loading The various acquisition devices are the following: Number of SmartGonioTM 0 0 1 2 Number of Monochromators 32 12 6 0 XRD System NO YES YES YES Instrument Type Simultaneous Simultaneous Sim / Seq Sim / Seq The two, three, four or five displays of the instrument inform the user about the spectrometer status, X-ray tube conditions and the monochromators, goniometer and or diffractometer status with all parameters regarding the measured element or compound line. The yellow pyramid located on top of the instrument is the “X-ray on” signal. This lamp is illuminated when the X-ray power supply is on. The red button is used to switch off the main power supply in emergency cases, while the green button allows the instrument to be powered. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-1 Chapter 3 INSTRUMENT DESCRIPTION Views of the ARL 9900 INTELLIPOWER Series Instrument Front view with 12 Position Sample Changer 1 1 2 3 4 X-Ray ON lamp Emergency Stop push-button Restart push-button 12 positions cassette loader Loading position Displays 4 5 2 5 6 6 3 Figure 3.1 3-2 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Front View with the X-Y Sample Changer 1 1 2 X-Ray ON lamp Emergency Stop push-button Restart push-button Display X-Y Cassettes / sample loader Right cover (closed) Left cover (closed) 7 6 5 2 4 3 3 4 5 6 7 Figure 3.2 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-3 Chapter 3 INSTRUMENT DESCRIPTION Back View of the Instrument 1 1 2 3 X-Ray ON lamp Top covers Bottom covers Venting apertures ACS connector Breakers and accessory plug Backside 2 4 5 6 3 5 6 4 Figure 3.3 On the back side of the ARL 9900 INTELLIPOWER Series instrument, as shown in Figure 3.4 the following features are available: 1. The connector for the computer - instrument link (ACS Link). 2. Reserved connectors 3. The main breaker (32 A) for the X-ray tube power supply. Note: With the mid power version (ARL 9900 INTELLIPOWER) this breaker is used like a switch, to turn on/off the generator. 4. The main breaker (16 A) for the electronic. 5. Accessory plug dedicated to the computer system. Maximum power current 3.15 A. 6. The Master Reset switch. It can be reached with a small screwdriver; insert it and press. 3-4 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION 6 1 1 MASTER RESET ACS LINK SERVICE LINK AC S LINK SERVI CE LIN K EXTENSI O I/O N Chapter 3 ACS connector Reserved connectors 32 A Breakers 16 A Breakers Accessory plug 3.15 A Master Reset 2 3 4 5 6 MA STER RESET 2 EXTENSION I/O COMPUTER 3A MAX X-RAY GENERA TOR MA IN 3 COMPUTER 3A MAX X-RAY GENERATOR MAIN 4 circuit breaker 5 Figure 3.4 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-5 Chapter 3 INSTRUMENT DESCRIPTION Instrument Display The ARL 9900 INTELLIPOWER Series instrument is equipped with a display. Three, four or five lines give messages about the spectrometer status, X-ray tube conditions and goniometer status. The next figure shows an example of the display, with one goniometer, one XRD channel, just after switching on the power. 1 ---- STAND BY ---90.00 3 1 LIF200 C1 2 Spectrometer and monochromators status X-ray tube status Goniometer 1 status Goniometer 2 / XRD status 20 kV 20 mA PARKED 3 4 2 4 Figure 3.5 Spectrometer Status Display The spectrometer status display shows the state of the ARL 9900 INTELLIPOWER Series instrument. The following list gives the messages and their meanings. Some messages appear simultaneously or alternately on the display. RESET INIT NOT CONFIGURED STAND BY MEASURE ANA 3 LOAD 3 EVAC 3 SEEK 3 F1 F2 F3 F4 PUMPING VENTING He HS : ON HS : OFF WAIT ACO The spectrometer is being reset. The spectrometer is being initialized. The spectrometer needs to be configured. Configuration data have to be downloaded from the ACS. The spectrometer is ready to analyse. The spectrometer is measuring. The cassette 3 is in analysis position. The cassette 3 is being loaded. The cassette 3 is being unloaded. The spectrometer is searching for the cassette in position number 3. The primary beam device 1(filter or collimator) is selected (if this option is fitted). The primary beam device 2 (filter or collimator) is selected (if this option is fitted). The primary beam device 3 (filter or collimator) is selected (if this option is fitted). The primary beam device 4 (filter or collimator) is selected (if this option is fitted). The spectrometer is being pumped down. The spectrometer is being vented. The Helium environment is selected. The Helium Shutter is on. The Helium Shutter is off. The instrument is waiting for analytical conditions. The sample rotation is on. 3-6 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 X-ray Tube Status Display The X-ray tube status display gives the kilovolts and the milliamps of the tube and some other information about the power supply state. The following list gives the messages and their meanings. RESET 60kV 40mA 50->30kV 50->80mA 30kV 80mA WAIT TOL The spectrometer is being reset. The X-ray tube settings are 60 kV and 40 mA for example. The X-ray tube conditions are changing from 50kV/50mA to 30kV/80mA. The X-ray tube conditions are 30kV/80mA and the spectrometer is waiting to be within the Tolerance. 50->40kV 50->20mA ECO The Eco mode is activated and the X-ray power supply is going to power down to 40kV/20mA. See Eco mode function described in this chapter. The Eco mode is activated and the X-ray power supply is in stand by at 40kV 20mA ECO 40kV/20mA. See Eco mode function described in this chapter. Goniometer Status Display The goniometer status display informs the user about the crystal, detector and collimator selection. It also shows the intensity currently being measured. Some messages can appear simultaneously or alternately on the display. ZERO REQUIRED CuKα III IIIII IIIII E4 45.03 III IIIII IIIII E4 CuKα FPC C4 20s 45.03 FPC C4 20s CuKα 45.03 LIF200 C4 LIF200 C4 The goniometer must be initialised. The count rate on the line CuKα is 2.6 104 counts or 26 kcps. The count rate on the angle 45.03° is 2.6 104 counts or 26 kcps. The angle of the CuKα line is 45.03° and the detector selected is FPC with the fourth collimator (fine). The remaining measuring time is 20 seconds. 20s 20s The angle of the CuKα line is 45.03° and the crystal selected is LiF200 with the fourth collimator (fine). The remaining measuring time is 20 seconds. Some other messages appear during the zero operation of the goniometer and inform the user about the current operations. XRD goniometer Status Display The XRD goniometer status display informs the user about the compound that is presently analysed. It also shows the intensity currently being measured. Some messages can appear simultaneously or alternately on the display. The goniometer must be initialised. ZERO REQUIRED 4 CaO_free III IIIII IIIII E4 The count rate on the line CaO_free is 1.2 10 counts or 12 kcps. 4 130.75 III IIIII IIIII E4 The count rate on the angle 130.75° is 1.2 10 counts or 12 kcps. CaO_free 20s The 2 θ angle for CaO_free line is 130.75° The remaining measuring time is 20 130.75 20s seconds. Some other messages appear during the zero operation of the goniometer and inform the user about the current operations. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-7 Chapter 3 INSTRUMENT DESCRIPTION Inside the ARL 9900 INTELLIPOWER Series instrument Instrument View This section describes the features and devices located inside the ARL 9900 INTELLIPOWER Series. Some devices are optional and may therefore not be fitted on your instrument. The following figure shows a general view of the instrument equipped with the SmartGonioTM and MultichromatorsTM. Vacuum Tank SmartGonio™ Sample in Analysis Position Sample Changer X-ray Tube Fixed Channels Molecular Pump Rotary Vacuum Pump Electronic Module Primary Beam device Generator Water Cooling + Heat Exchanger Figure 3.6 The main parts of the instrument are listed bellow: Spectrometer tank with analytical devices The analytical devices like Fixed Channels, Goniometer, Diffraction System (XRD) and Primary Beam Devices (PBD) are located in the thermal controlled vacuum tank. The analytical devices are mounted concentric around the sample. Sample introduction Different sample magazines allow unattended operation, prepare the sample for introduction into the Primary Chamber and finally move it into the analytical position where sample rotation is possible. Analytical environment Environment (vacuum or air) in the Spectrometer tank, thermal regulation of the instrument and the analytical devices, gas regulation for the detectors. Sample excitation X-ray tube, X-ray tube power supply, X-ray tube cooling system. Electronic devices Electronic rack and boards, main power connections, power distribution for the main and for low voltage p.s. 3-8 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 The following figure shows a general view of the 9900 INTELLIPOWER Series WORKSTATION equipped with Full Diffractometer Channel. Spectrometer tank XRD Detector Rotation Sample changer Sample conveying system Detector XRF tube X-ray tube X’trA optics XRD Tube Rotation Gas regulation Molecular Pump Electronic Module Rotary Pump X-Ray Power Supply XRD tube Figure 3.7 XRD Power Supply X-RAY TUBE Cooling System AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-9 Chapter 3 INSTRUMENT DESCRIPTION The following figure shows a general view of the instrument equipped with the Full Difractomer and a SmartGonioTM. Up to 6 mono or 1 SmartGonio XRD tube Up to 6 mono or 1 SmartGonio XRD Detector Figure 3.8 Possible configurations: Number of SmartGonioTM NO NO 1 2 NO NO NO Number of Universal Goniometers NO NO NO NO 1 1 2 Number of Monochromators 30 12 6 0 22 14 0 Compact XRD NO NO NO NO NO YES NO Full XRD Instrument Type Simultaneous Sim / Seq Sim / Seq Seq Sim / Seq Sim / Seq Seq NO YES YES YES NO NO NO 3-10 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Electronic Rack All electronic boards take place in this rack. Figure 3.13 shows the location and the name of each board. Extention rack Extention rack Basic rack XQIM : X-ray Quantometer Master XPS : X-Ray Spetrometer power XCM : X-ray Cassette Magazine XSI : X-ray Sample Introduction XDI : X-ray Detector Interface XDI : X-ray Detector Interface XGT : X-ray Gas and Thermal XSH : X-ray Sample Handling or 8 9 10 8 9 10 1 2 3 4 5 6 7 8 9 10 KXx9815D00300 Figure 3.9 The XSH board and XCM board are never fitted both together. XDI : X-ray Detector Interface Goniometer/XRD board Goniometer/XRD board Goniometer/XRD board AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-11 Chapter 3 1. XSI INSTRUMENT DESCRIPTION X-Ray Sample Introduction. This board does control the sample loading from the atmospheric environment to the analytical position and reverse. X-ray Quantometer Master. This board is the interface with the computer and it manages all sample movements except those done by the sample changer. It drives also the primary beam filter and the programmable aperture changer. This electronic board is the power interface between the XQM and its devices. X-ray Gas and Thermal. This electronic board monitors the FPC gas regulation and the thermal regulation of the spectrometer. Not used X-ray Handling Interface. This electronic board drives the large sample changer. X-ray Cassette Magazine. This electronic board drives the 12 position sample changer. Not used X-ray Goniometer Board. This electronic board drives the goniometer crystal and detector assembly movements, the crystal heating, (the collimator changer, the crystal changer, for Goniometer F45), and generates the detectors high voltage. X-ray Goniometer Board. This electronic board drives and controls the goniometer detector assembly movements, the X-Ray tube assembly movements, the crystal heating and generates the detector high voltage. X-ray Detector Interface. This electronic board counts the number of photons received by the goniometer detectors. X-ray Monochromators Interface. These boards are located inside the vacuum tank. They control all activities dedicated to the fixed channels. 2. XQIM 3. XSP 4. XGT 5. 6. XHI 7. XCM 8. 9.a XGBI Universal Goniometer TM F45 or SmartGonio 9.b XGBD XRD Channel 10. XDI 11. XMI Remark: When two or more Goniometers/XRD Channels are installed into the vacuum tank, a special extension electronic rack is added to the basic one at its left hand side. This additional rack does include one XGB/XGBM and one XDI per Goniometer/XRD. 3-12 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Analytical Conditions The sample can be measured using different conditions like filters, vacuum environment, different crystals or detectors etc. This section describes these different parts. Goniometer The goniometer is the sequential acquisition device of the ARL 9900 INTELLIPOWER Series instrument. The goniometer is a fully automatic, gearless, microprocessor controlled device on which crystals, detectors and collimators are arranged to satisfy Bragg’s law (nλ = 2d sinθ) and to cover the needs of various applications. The two encoder systems ensure fully independent positioning for both the crystal and the detector. The goniometer is used to perform analyses and scans. Analysis is performed by positioning the crystal at a given Theta and the detector at 2 Theta and counting for certain amount of time. Then the crystal and detector are rotated to a different angle for another line etc. Scanning can be performed by selecting a small angular increment and a short time measuring time per step. The instrument can be either equipped with the universal F45 Goniometer or with a SmartGonio™. The Universal F45 Goniometer The universal goniometer can be fitted with up to nine crystals, one or two detectors and up to four collimators. The figure below shows such a goniometer. 1 1 Collimator changer Crystal changer FPC detector SC detector 2 2 3 3 4 4 KXx9460D00100 Figure 3.10 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-13 Chapter 3 Configuration table INSTRUMENT DESCRIPTION It is very important to choose the right combination of collimator, crystal and detector for your analysis needs. The following tables will help you doing this: FEATURE K Spectra L Spectra COLLIMAT. X-Coarse 2.6° Coarse 0.6° Medium 0.25° Fine 0.15° CRYSTAL AXBeB AX20 AX16 AX09 AX06 TlAP ADP PET InSb Ge111 LiF 200 LiF 220 LiF420 DETECTOR FPC Scintillation Sensitivity Resolution Elements Be B C N O -F -Na Mg Al Si P -S -Cl K Ca...Ti…Fe Co...Zn…Sn Sn...Yb Hf...U V.High High Good Low High Good High Good High Good Low Good High Good Good Fair Low Low Fair Good High Low Low Low Low Low Good High Fair High High Good High V.High Be B C N O O Mg Al Si P K Ti Zn Note: The hatched ranges indicate that the application is possible, but not optimum for the concerned elements. 3-14 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION The SmartGonio™ Chapter 3 The SmartGonio™ is fitted with three crystals, two detectors and one collimator. The figure below shows a SmartGonio™. 4 1 1 2 SC detector FPC detector Crystal changer Collimator 3 2 3 4 Figure 3.11 Configuration table The following table shows the fixed configuration of the SmartGonio™: Note: FEATURE K Spectra L Spectra The collimator will be selected and installed according to your application. Sensitivity Resolution F Na Mg Al Si P S Elements Cl K Ca...Ti…Fe Sn.……..Yb Co...Zn…Sn Hf……….U COLLIMATOR Coarse 0.6° High Medium 0.29° Good Fine 0.17° Low CRYSTAL AX06 PET LiF 200 DETECTOR FPC Scintillation High Good Good Fair Good High Low Fair Good Zn Fe Figure 3.12 Note: The hatched ranges indicate that the application is possible, but not optimum for the elements concerned. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-15 Chapter 3 INSTRUMENT DESCRIPTION Compact XRD diffractometer Unique integrated phase analysis XRF analysis determines the elemental composition of a sample, but mineralogical information is only available through X-ray diffraction (XRD). It permits analysis of the phases or compounds in crystalline materials, e.g. rocks, minerals, oxide products, etc. As an example, XRF only measures the total Ca concentration in a sample, while XRD can give information about the CaO, CaCO3 and Ca(OH)2 contents. Generally, separate XRD equipment is required to obtain qualitative and quantitative structural data. When both types of analysis are required, two separate X-ray instruments should be maintained and operated, which results in significant costs for the user. The integration of an innovative X-ray diffraction system allows both techniques to be fitted into the same ARL 9900 Series instrument. This patented diffraction system is capable of making qualitative scans and quantitative analysis thanks to its Moiré fringe positioning mechanism. Closely coupled diffraction optics produce very high sensitivity; they offer opportunities for new applications, ensuring a high stability of analysis. Sample alignment problems, common in Diffractometry, are avoided thanks to the accurate sample positioning and focusing beam X-ray geometry. This allows covering a wide 2d range, with an angular range from 85° to 144° with the Compact XRD system. Separate data sheets are available describing the advantage of such a combined instrument applied to process monitoring in many industries such as cement (Total Cement Analyzer), iron & steel (Total Iron X-ray Analyzer), aluminum (Total Aluminum X-ray Analyzer) as well as other mining processes involving iron ores, limestone, slags, sinters and beach sands among others. Motor XRD System Cristal X-Ray Tube Rotation Detection Primary Collimator Encoder Sample Cassette Primary Beam Device Figure 3.13 3-16 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Full XRD diffractometer The integration of an innovative X-ray diffraction system allows both techniques to be fitted into the same ARL 9900 Series instrument. This patented diffraction system is capable of making qualitative scans and quantitative analysis thanks to its Moiré fringe positioning mechanism. Closely coupled diffraction optics produce very high sensitivity; they offer opportunities for new applications, ensuring a high stability of analysis. Sample alignment problems, common in Diffractometry, are avoided thanks to the accurate sample positioning and focusing beam X-ray geometry. This allows covering a wide 2d range, with an angular range from 10° to 70° with the Full XRD system. XRF tube Detector X’trA optics Sample XRD tube Figure 3.14: View of the ARL 9900 Workstation Series The Diffractograms can be visualised and worked out with OXSAS or with third party software Visual Crystal,... See example below: AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-17 Chapter 3 OXSAS Diffractograms. INSTRUMENT DESCRIPTION Figure 3.15 Visual CRYSTALR Diffractograms of a ground sample (rock and clay). Figure 3.16 3-18 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Primary Beam Filter (Option) The primary beam filter (PBF) is inserted between the tube and the sample to modify the X-ray excitation. If XRD channel is not present, four different Primary Beam Filters could be installed on the Primary Beam Device mechanism. List of Primary Beam Filters (Option) Filter type Cu 0.25mm Name on the display F1 Use For analysis of Ru, Rh, Pd, Ag and Cd (elements that are interfered by Rh lines emitted from the X-ray tube Rh anode) in light and variable matrices. To improve the peak to background ratio of NiKα and CuKα lines. To improve the peak to background ratio of PbLα, PbLß and AsKα, AsKß lines in light matrices. This filter is a protection shield against dust coming from the sample. (Mainly not used on ARL 9900 INTELLIPOWER Series) Fe 0.01mm Al 0.5mm Be 0.127mm F2 F3 F1 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-19 Chapter 3 INSTRUMENT DESCRIPTION Fixed channels High-throughput elemental analysis is ensured via fixed channels, each dedicated to the analysis of one element. New, compact slit-crystal geometry has been developed which optimizes the sensitivity and spectral background levels in order to obtain the lowest limits of detection. New detectors ensure a wider linearity of response permitting to reach very high precision levels for major element analysis. Up to 32 monochromators can be fitted in the high power ARL 9900 INTELLIPOWER NEXRD series instruments. Configuration of the monochromators The monochromators are fixed assemblies of three elements satisfying BRAGG’s law (nλ = 2d sinθ), a crystal, a detector and a focalization or collimation system. There are two distinct types of monochromators. Monochromators equipped with focusing crystals: X-ray tube Focussing crystal Detector slit Source slit Secondary beam Primary beam Sample Detector Figure 3.17 Natural crystals such as LiF, ADP or PET allow for the utilization of curved crystal focalizing systems of great precision and resolution. These natural crystals ensure excellent analytical results for elements from magnesium atomic number 12 and higher. The crystals used by Thermo on ARL instruments are curved to a perfectly focusing geometry and aligned on a narrow primary slit thus ensuring very good analysis resolution. The choice of crystal is made according to its reflection capabilities for the wavelength of the element to be analyzed. Various types of gas detectors or scintillation counters are used according to their measurement efficiency for the wavelength of the element to be analyzed. Monochromators with curved multilayer crystals and gas sealed detectors are also available for Na and Mg. 3-20 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Monochromators equipped with flat crystals (Multilayers) Chapter 3 X-ray tube Crystal θ θ 2θ Secondary collimator Primary collimator Primary beam Sample Secondary beam Flow proportional counter Figure 3.18 The Multilayers are very efficient reflectors for soft X-rays and permit excellent analysis results of light elements from Boron to Magnesium. The physical characteristics of Multilayers, favor the use of flat crystals arrangement equipped with Soller collimators and gas flow detectors (Ar/CH4) with extremely thin windows which are transparent to soft rays. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-21 Chapter 3 INSTRUMENT DESCRIPTION Analysis Environment Environment Setting Two different modes can be selected, either with a dedicated menu function, or as a step of operation in the unattended analysis mode. Vacuum Atmosphere This is the environment used for the measurement of all samples that are safe in vacuum (e.g. solids and pressed powders). This mode does vent the spectrometer tank and is only used for maintenance purpose. Remark: The typical spectrometer tank pressure in vacuum environment is around 2 Pa (0.00029 PSI) Gas Regulation (Optional) The ARL 9900 INTELLIPOWER Series requires one type of gas: Argon-Methane (P10 gas) for the flow proportional counter (FPC). This detector is installed on the goniometer and on some monochromators. The gas regulation system is controlled by the XGT board. In addition to these functions this electronic board drives the venting valve of the tank, checks the vacuum safety in order to prevent any X-ray leaks and controls the thermal stability. Thermal Regulation The ARL 9900 INTELLIPOWER Series instruments are designed to provide stable results on long term. To satisfy to this request the instrument must as well show a long term thermal stability. Therefore components which are generating heat have been located into a non thermal controlled area. On the other hand, all the components that need to have a precise thermal stability have been located into a thermal controlled and insulated area. 3-22 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Sample Excitation The sample excitation is based on end window X-ray tube which is energised by a solid state power supply. The X-ray tube cooling system is assumed by a water circuit. In order to prevent any problem with the Xrays or high voltage, the instrument is equipped with a safety interlock system. X-ray Tube The X-ray tube is positioned at 90° relative to the horizontal plane and the distance between the anode and the sample surface is 30 mm. The end window design allows a very high sensitivity for light elements and thus low limits of detection. Light element analysis is very efficient with the 75 micron (50 micron optional) beryllium window having a low absorption on light elements wavelengths. The usual target is Rhodium. X-ray tube Primary X-ray beam Figure 3.19 X-ray Power Supply The X-ray power supply is a solid state generator that delivers a maximum power depending of your configuration (1200, 3600 or 4200 Watt). This unit controls the high voltage and the current applied to the tube. The voltage can be selected by steps of 1 kV. The current can be selected by steps of 1 mA with some restrictions if the voltage selected is lower than 20 kV because it is physically not possible to get for example 0 kV / 120 mA. With the following formula the maximum current according to the desired high voltage can be calculated: Imax = 4 26 ∗ kV + 5 ∗ kV 2 100 ( ) AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-23 Chapter 3 Where: Imax is maximum current authorized kV is the desired kilo Volt Examples: kV desired I maximum 0 kV 5 kV 0 mA 10 mA kV desired 10 kV 25 kV I maximum 30 mA 120 mA INSTRUMENT DESCRIPTION The X-ray power supply can be supplied in different versions. Instrument ARL 9900 INTELLIPOWER 1200W ARL 9900 INTELLIPOWER 2500W ARL 9900 INTELLIPOWER 3600W ARL 9900 INTELLIPOWER 4200W Maximum Power 1.2 kW Maximum Voltage 60 kV Maximum Emission Current 60 mA 2.5 kW 60 kV 100 mA Standard 3.6 kW 60 kV 120 mA Option Standard 3.6 kW 4.2 kW 70 kV 60 kV 120 mA 120 mA Option 4.2 kW 70 kV 140 mA Ecological Mode The ecological mode (Eco Mode) is a function which allows you to lower the power consumption and to increase the life time of the X-ray tube. Warning: It is strongly recommended to never completely switch off the X-ray tube power supply. A frequent shut down and powerup does lead to destruction of the X-ray tube. When the instrument is idle for a pre-defined time the power is reduced to a stand-by value. For example, if the working condition is 50 kV and 50 mA and the instrument has been idle for 1 hour the power will be reduced to 40 kV and 20 mA in 30 minutes. As soon as the user starts a new measurement the required working condition will be reached automatically. Another function is available to program the time to raise the X-ray tube to a certain working condition. This can be helpful if the instrument needs to be stabilised before the analysis is started. For example, the X-ray tube is at 40kV/20mA during the night and in the morning it is raised to 50kV/50mA 1 hour before the user arrives in the lab. 3-24 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 X-ray Tube Safety Interlock All panels or covers with one of the signs shown in Figure 3.20 are controlled by an interlock system. If these panels or covers are not in place, the interlock system will disallow switching on the power on the Xray tube. We strongly recommend the user to contact our office if the user needs to remove these protections. High voltage Radiation Figure 3.20 Note: This safety interlock operates only on the X-ray tube power supply. The emergency stop button will switch off the instrument main voltage power supply. X-ray Tube Cooling System for ARL 9900 INTELLIPOWER Series 3600W and 4200W The cooling of the X-ray tube is achieved with an internal closed circuit using de-ionised water, which in turn is cooled through a heat exchanger which uses either tap water or water cooled through a water chiller. X-ray Tube Cooling System for ARL 9900 INTELLIPOWER Series 1200W 2500W The cooling of the X-ray tube is assured by an internal closed circuit which is cooled through an air-water heat exchanger. Next figure shows the air-water heat exchanger. 2500W 1200W Figure 3.21 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-25 Chapter 3 INSTRUMENT DESCRIPTION Sample Handling Systems The sample handling is undertaken by two main devices: ♦ The sample changer. It brings the cassette or the sample holder or onto the lift. ♦ The primary chamber: It serves as an air lock between the atmospheric pressure and the vacuum environment. The lift brings the cassette into the primary chamber and then the sample is moved in the analysis position. Three versions of sample loading systems are available: ♦ Manual sample loading ♦ Sample loading with 12 position sample changer ♦ Sample loading with large X-Y sample changer Manual sample loading The figure below shows a detailed view of the loading position for an instrument with manual sample loading. Manual loading position Figure 3.22 3-26 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Sample loading with 12 position sample changer Chapter 3 This sample loader (see figure below) is designed to receive up to 12 standard cassettes. The positions of the sample changer are coded and the loading time is minimized thanks to its bi-directional concept. Figure 3.23 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-27 Chapter 3 Large X-Y sample changer INSTRUMENT DESCRIPTION This sample loader is a large capacity magazine. It can load standard cassettes and/or it is able to load the samples directly into the ARL 9900 INTELLIPOWER series instrument using special sample supports. Three versions are available: ♦ 98 cassettes for samples of maximum height 30 mm and maximum diameter 52 mm. Figure 3.24 Cassettes version composed of: Load position 1 7 0 101 107 • 2 trays of 49 positions. • 1 clamp for the cassettes. 43 Tray 0 samples 1..49 49 143 149 Tray 100 samples 101..149 Figure 3.25 3-28 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 ♦ 98 samples which can be loaded directly into the ARL 9900 INTELLIPOWER using special sample supports. Figure 3.26 Load position 1 7 0 101 107 Samples version composed of: • 2 trays of 49 positions. • 1 clamp for the ∅ 57mm support. • Support for the samples families diameter of: 30.5 to 32mm. 32 to 35 35 to 41 41 to 50 Samples must have parallel faces (+/-2 mm tolerance for 52 mm ∅) See figure 3.28 43 Tray 0 samples 1..49 49 143 149 Tray 100 samples 101..149 Figure 3.27 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-29 Chapter 3 ♦ OEM X-Y Sample Loader INSTRUMENT DESCRIPTION The OEM (Original Equipment Manufacture) X-Y Sample Loader has been designed in order to connect an ARL 9900 INTELLIPOWER series spectrometer to an automatic sample preparation station generally for pressed powders through transport belt(s). It was conceived and developed for our main OEM Engineering Company customers. These companies integrate the ARL 9900 INTELLIPOWER series instrument with OEM X-Y Sample Loader into their own developed Computer Based Automation Systems for on-line use. 1 7 0 6xx 6xx Waiting positions Load position Belts positions 7xx 43 Tray 0 samples 1..49 49 7xx 7xx Baskets positions 5xx Waiting positions 6xx 6xx 0 1 7 Load position 5xx Belts positions 7xx 7xx 7xx Baskets positions Tray 0 samples 1..49 43 49 Figure 3.28 Transport belt(s) and docking port The OEM X-Y Sample Loader takes samples from a conveyor belt and loads them automatically into the instrument. The samples are generally powders which are pressed into steel rings. A second belt can be installed for unloading samples or to load a second type of samples (e.g. fusion beads). The docking port accepts one or two conveyor belts of typical 50 to 80 mm width. The belt(s) can be fitted on the loader either to the left front or back, or to the right front or back (see figure 3.27). The belt surface must be positioned at 978 mm from the floor. Note: If the sample is fetched with the clamp on a belt installed on the left back position, the belt position will show an angle of about 15° relative to the left side of the X-Y loader (see figure 3.27). 3-30 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 9900 OEM X-Y LOADER CLAMP RIGHT, SUCTION PAD LEFT D 68.00 Sample Free zone for clamp 36.00 970.00 98.00 min. Clamp 222.00 1220.00 183.00 min. Suction pad 336.00 978.00 Clamp area 115.00 3.00 145.00 930.00 145.00 For suction pad only 428.00 144.00 min. Clamp 222.00 978.00 Suction pad area 59.00 min. Suction pad Figure 3.29 Disconnection of the X-Y sample loader from the instrument is required for annual maintenance. Therefore the X-Y loader side apertures are wide enough to permit the belts to stay in there location. Suction option This option makes possible the handling of the samples of different diameter coming from belts. Some restrictions on dimensions of the samples must be taken into account: 34.00..52.00 mm N6 max. 2.20° (max. 2mm for diam. 52mm) 4.00..25.00 mm Figure 3.30 The maximum height of the samples used with the trays is 25 mm and their weight should not exceed 200 g. For other dimensions, the cases must be treated individually through a request for speciality. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-31 Chapter 3 Automation INSTRUMENT DESCRIPTION It is important to point out that in each of these systems there is a “Host” Computer supplied by the OEM Engineering Company. This computer is interconnected to the ARL 9900 INTELLIPOWER/OXSAS instrument to direct and control the samples input to the OEM X-Y Sample Loader, the analysis and the output to the transport belt or to classification boxes. The “Host” computer is in general also doing other tasks, like supervising the incoming of material to be analyzed through a pneumatic transport system or driving the automatic preparation machines. The OXSAS/OEM software option allows interconnection of the OEM software to our OXSAS software. Some development work is required from the OEM part such that their software takes control of our OXSAS software through this interconnection software module. The ARL 9900 INTELLIPOWER/OXSAS with OEM X-Y Sample Loader will function with the direction and control being performed by the “Host” Computer. Consequently we expect that only Engineering Companies or companies with engineering expertise will order an OEM X-Y Sample Loader. Automatic samples When loading pressed samples, they must be pressed in Herzog steel rings of diameter 40 mm x height 15 mm or diameter 51.5 mm x height 8.5 mm. On special request, automatic loading of fused beads coming from an automatic fusion unit can be adapted. In this case the fusion bead sample is taken from the belt by a suction device and deposited on an adaptation ring with the analysis face upward. The ring is then carried to the lift of the instrument. In case both types of samples are to be handled the fusion beads must have a smaller diameter than the steel rings. The fusion beads should be sent in advance to the Ecublens factory for evaluation. Manual samples, Setting-up, Control and Type standard samples (SCT) The OEM X-Y Sample Loader comprises usually 49 positions (up to 63 on option) for what we call SCT samples (which comprise setting-up samples (SUS), control samples and type standard samples) and for manual loading samples. After analysis these samples are brought back to their original position. Up to 2 waiting positions for automatic unloading to the conveyor belt(s) and up to 3 classification baskets for storing of automatic samples after analysis are available. Access to 49 of the 63 positions for manual loading or setting-up samples is done by opening the corresponding Plexiglas door of the loader and will not stop the automatic loading or unloading of a sample. The manual samples can be powders pressed into steel rings of the same diameter as the automatic samples. If other samples are required to be manually analyzed -for example fused beads or setting-up samples (SUS) - they must be mounted in holders to simulate a steel ring in its external diameter. The available holders can house samples of the following diameters: • 30.5 mm to 32 mm • 35 mm to 41 mm • 32 mm to 35 mm • 41 mm to 50 mm In the case when the manual samples have odd shapes or are very thin, special cassettes have been developed to be used in parallel to the automatic samples which are loaded without cassette. The drawback of working with such special cassettes is that the manual sample will be placed further away from the X-ray tube anode due to the thickness of the top of the cassette. Therefore calibration curves have to be adapted with the new geometry specifically for the samples that are analyzed in these cassettes. These cassettes can house samples of diameter max. 52 mm and height of max. 30 mm. They have an opening diameter of 31 mm (while the opening diameter inside the instrument is 29mm – the difference in diameter is such that the analysis devices will not see the edge of the cassette top in the analysis position). For smaller samples, special cassettes with gold or silver coating and opening of small diameter can be used but they can only be ordered with prior agreement of the XRF Product Manager. A special gripper must be fitted on the X-Y loader with the capability to grab both the sample coming on the belt and these special cassettes. 3-32 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION OXSAS / OEM software option Chapter 3 The full details of the direction and control which must be performed by the Host Computer are described in the ARL Manual P/N AA 83508-02 ARL OXSAS V3.2 “OEM Protocol Description”. This manual covers the messages that must be exchanged between OXSAS and a Host Computer associated with an Automatic System. A chapter of the OXSAS reference manual (Automation option system) describes how OXSAS can be used with such an Automation System -as supplied by one of our Engineering Company customers-. It also describes how to set OXSAS to operate in Automatic Mode and the features that are available when running in this mode. The OXSAS / OEM software option adds features to OXSAS that allow it to communicate with a Host Computer and to perform the analysis calculations and result distribution without any operator involvement. The message exchanges which are needed between OXSAS and the Host Computer are able to deal with the following cases: • Production Sample Analysis Messages cover Analytical Task, Sample Identification, Start Analysis • Return of Sample to Preparation Machine • Setting-Up Sample (SUS) Analysis • Control Sample Analysis • Type Standard Analysis These messages can be exchanged using a LAN-Local Area Network and the protocol TCP-IP. In its simplest form the Host Computer can perform the functions and message exchanges dealing only with Production Sample Analysis. In such a case all other operations (drift corrections, SPC by running control samples, type standardization) will have to be performed manually. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-33 Chapter 3 INSTRUMENT DESCRIPTION Sample holders Every sample must be placed in a sample holder before it can be introduced into the ARL 9900 INTELLIPOWER Series. The introduction of a sample without the correct holder will stop or damage the sample handling system. There are two different kinds of sample holders: ♦ Cassettes are used for handling any kind of solid and pressed powder samples. Large cassettes are used with 12 Position Sample Changer. Small cassettes are used with the X-Y sample changer and with the single position loading. ♦ Sample Adapters are used for handling samples without cassettes. 4 different families of sample diameters are defined for the large X-Y sample changer. In case of automation, the centring ring can be adapted to the production sample size and shape. Cassettes The standard cassette aperture is ∅ 29 mm and 31 mm. Special coated cassettes with smaller aperture can be obtained on request. The following picture describes the maximum sample size that can be used with each model of sample changer. φ 29 mm or φ 31 mm special Sample: maximum dimension φ 52 mm 36 mm KXx9880D00100 Small cassette Figure 3.31 Special cassette for Workstation φ 33 mm special Sample: maximum dimension 30 mm φ 52 mm 36 mm KXx9880D00100 Small cassette Figure 3.32 3-34 ARL 9900 INTELLIPOWER Series User Manual 30 mm AA83654 INSTRUMENT DESCRIPTION Chapter 3 φ 29 mm Sample: maximum dimension φ 60 mm Large cassette Figure 3.33 Special cassette for Workstation φ 33 mm Sample: maximum dimension φ 60 mm 50 mm Large cassette Figure 3.34 Centring rings In order to insure the sample to be centred, special rings with different diameters are available. 50 mm 40 mm 40 mm φ 32 mm φ 40.5 mm φ 36mm φ 31mm φ 22 mm 17 12 7 KXx9480D00200 Figure 3.35 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-35 Chapter 3 INSTRUMENT DESCRIPTION Sample supports With X-Y sample changer where cassettes are not suitable, the samples can be fitted into special sample supports. Depending upon the samples diameter, 4 different supports are available. For sample diameter ranges of: ♦ ♦ ♦ ♦ 30.5 to 32 mm 32 to 35 mm 35 to 41 mm 41 to 50 mm Figure 3.36 3-36 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION Chapter 3 Sample Loading System The following figure shows the principle of the sample loading system. Cassette and/or sample support Shutter Shutter motor Shell Spectrometer pumping line Transfer motor Primary chamber pumping line Loading lift motor Figure 3.37 Analysis lift motor Sample rotation motor ♦ Sample Changer ♦ Shutter ♦ Load lift ♦ Primary chamber It allows to move or to pick-up the desired cassette or sample support from a dedicated position with a numeric identification It serves as an air lock between the atmospheric pressure and the vacuum environment. It is the mechanism dedicated to transfer the cassette and/or the sample support from the sample changer into the primary chamber. It serves as an air lock between the atmospheric pressure and the vacuum environment. The lift drives the sample cassette or sample support into the primary chamber. It is the mechanism to move the sample from the loading lift to the analysis lift. It is the mechanism to raise the sample cassette or sample support to the analysis position under the X-ray tube beam The sample rotation motor spins the cassette at 30 revolutions per minute during the analysis time in order to average the counts in case the sample is not homogeneous or when the sample presents surfacing grooves. ♦ Transfer ♦ Analysis lift ♦ Sample rotation AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-37 Chapter 3 INSTRUMENT DESCRIPTION Sample Loading Process The ARL 9900 INTELLIPOWER NEXRD Series is designed to analyse solid samples. These samples can be inserted into a cassette or can be put onto a sample support for analysis. The analysis of the samples is done under vacuum. The sample is first loaded into the primary chamber which is under air. The shutter closes and the primary chamber is pumped down to a low pressure. The sample is then transferred to the spectrometer and raised to the analytical position, as explained hereafter. ♦ Step 1 Next figure shows the instrument ready to load a sample. The sample changer brings the desired sample onto the load lift. Moving Parts Structure Parts Washer Parts Vacuum Air Spectrometer Tank Spectrometer pumping line Primary chamber pumping line Figure 3.38 3-38 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION ♦ Step 2 The load lift moves the cassette and/or the sample support into the shell (see movement ‘a’). Moving Parts Structure Parts Washer Parts Vacuum Air Spectrometer Tank Chapter 3 a Spectrometer pumping line Primary chamber pumping line Figure 3.39 ♦ Step 3 The shutter is closed (see movement ‘a’). Moving Parts Structure Parts Washer Parts Vacuum Air a Spectrometer Tank Spectrometer pumping line Primary chamber pumping line Figure 3.40 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-39 Chapter 3 ♦ Step 4 INSTRUMENT DESCRIPTION The primary chamber is then evacuated to a low pressure by the vane stage pump (see action ‘a’). Moving Parts Structure Parts Washer Parts Vacuum Air Spectrometer Tank a Primary chamber pumping line Spectrometer pumping line Figure 3.41 ♦ Step 5 When the required vacuum is reached, the lift moves further down pulling the ring down to free the shell (see movement ‘a’). Moving Parts Structure Parts Washer Parts Vacuum Shell Air Spectrometer Tank Ring a Spectrometer pumping line Primary chamber pumping line Figure 3.42 3-40 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION ♦ Step 6 Chapter 3 The shell and cassette and/or sample support are moved out of the primary chamber by the transfer mechanism (see movement ‘a’). Moving Parts Structure Parts Washer Parts Vacuum Air Spectrometer Tank a Spectrometer pumping line Primary chamber pumping line Figure 3.43 ♦ Step 7 The cassette and/or the sample support are then transferred into the spectrometer (see movement ‘a’). Primary chamber Spectrometer Tank a Spectrometer pumping line Moving Parts Structure Parts Washer Parts Vacuum Air Figure 3.44 AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-41 Chapter 3 ♦ Step 8 INSTRUMENT DESCRIPTION As soon as the shell is under the analysis position, the analysis lift raises the cassette and/or the sample to the analysis position (see movement ‘a’). Primary chamber Spectrometer Tank Spectrometer pumping line Moving Parts Structure Parts Washer Parts Vacuum Air a Figure 3.45 ♦ Step 9 (Sample in Cassette) The sample is raised to the analysis position by the analysis lift. The sample rotation spins (see movement ‘a’) and the analysis sequence started. a Primary chamber Spectrometer Tank Spectrometer pumping line Moving Parts Structure Parts Washer Parts Vacuum Air Figure 3.46 3-42 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT DESCRIPTION ♦ Step 9 (Sample without Cassette) Chapter 3 Warning: with a 12 position sample conveyor or an X-Y magazine of cassette type, do never load a sample without cassette or with a sample support. The figure below shows a sample in the analytical position placed on an adapter ring. The spectrometer lift moves the sample up into the analysis position. This movement is controlled by a sensor and therefore allows variable sample thickness. The lift can compensate for a 2 mm non-parallelism of samples. The sample is raised to the analysis position by the analysis lift. The sample rotation spins (see movement ‘a’) and the analysis sequence started. Sample Dummy cassette Primary chamber Spectrometer Tank Adaptation ring a Ball bearing for sample rotation Spectrometer pumping line Moving Parts Structure Parts Washer Parts Vacuum Air Figure 3.47 At the end of the analysis period, the rotation is stopped and the sample cassette or sample support is unloaded following the reverse sequence and driven back to its original position. AA83654 ARL 9900 INTELLIPOWER Series User Manual 3-43 4 INSTRUMENT PREPARATION INSTRUMENT PREPARATION Chapter 4 4 INSTRUMENT PREPARATION Switch on the Instrument Note: At this level we assume the ARL 9900 Intellipower Series instrument is properly installed, the main power, the water, gas, serial interface, computer, video terminal and printer are properly connected. On the back side of the instrument: 1. Switch MAINS breaker on. 2. Switch X-RAY GENERATOR breaker on. MASTER RESET ACS LINK SERVICE LINK MAST ER RESET ACS LINK SERVICE LINK EXTENSI ON I/O EXTENSION I/O COMPUTER 3 A MAX X-RAY GENERATOR MAIN COMPUTER 3A MAX X-RAY GENERATOR MAIN KXx9800D01600 1 1 Circuit breaker Figure 4.1 AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-1 Chapter 4 INSTRUMENT PREPARATION With 12 positions cassette magazine 3. On the front of the instrument, turn the red emergency stop button (2) clockwise on. 4. Press the green start button (3) 1 1 2 3 4 X-Ray ON lamp Emergency Stop push-button Restart push-button 12 positions cassette loader Loading position Displays 4 5 2 5 6 6 3 Figure 4.2 Monitor the left upper display. As –NOT CONFIGURED- is displayed, the instrument data need now to be downloaded from the computer system. Follow the instruction of the next section. 4-2 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION Chapter 4 With X-Y magazine 3. On the front of the instrument, turn the red emergency stop button (2) clockwise on. 4. Press the green start button (3) 1 1 2 X-Ray ON lamp Emergency Stop push-button Restart push-button Display X-Y Cassettes / sample loader Right cover (closed) Left cover (closed) 7 6 5 2 4 3 3 4 5 6 7 Figure 4.3 Monitor the left upper display. As –NOT CONFIGURED- is displayed, the instrument data need now to be downloaded from the computer system. Follow the instruction of the next section. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-3 Chapter 4 INSTRUMENT PREPARATION Switch on the PC Make sure the computer system is plugged to the main power supply. Switch on the computer unit, the video terminal unit and the printer. Once Windows XP is started, in the desktop double click on the icon to start the user interface software. Start up procedure with OXSAS software. On the desktop double click on the OXSAS icon to start the software. Enter the User name and Password Figure 4.4 In User Name box enter !USER! Leave the Password box empty Click OK Or In User Name box enter !MANAGER! Leave the Password box empty Click OK Important: For security reasons, we strongly recommend to provide real passwords for these default accounts and to create own accounts for your staff with there dedicated passwords. Please refer to the OXSAS online help for more details. 4-4 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION Chapter 4 Instrument Configuration and Initialisation Instrument Initialisation On the main toolbar select Tools, Actions and Send Instrument Configuration Figure 4.5 In the next box check High voltage calibration, Position Calibration, Instrument Status and click OK Figure 4.6 The instrument configuration is now downloaded. The following information will appear on the instrument display. STAND BY kV : 0 mA : 0 ZERO REQUIRED Figure 4.7 The initialisation of the instrument is done to reset all microprocessors and the mechanical parts. In case of problem with the instrument this operation should be done. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-5 Chapter 4 INSTRUMENT PREPARATION Perform a goniometer initialisation as described below. On the main toolbar select Tools, Actions and Zero Goniometer Figure 4.8 Select the goniometer to be initialised Figure 4.9 Valid the question Are you sure you want to reset the goniometer with OK The goniometer initialisation process can be monitored on the instrument goniometer display. At the end of the zero process the crystal, detector, collimator, the angular position. Gas Supply Argon-Methane Gas for FPC Check that the gas bottle tap is open. Check that the pressure is set at 0.25 bars on the bottle pressure reducer. The argon-methane gas flow should be set to 6 ml / min. and the regulation pressure must be 105500 Pa. to be sure the gas regulation system works properly it is recommended to check the gas status. 4-6 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION On the main toolbar select Tools, Actions and read Status Chapter 4 Figure 4.10 In the next window select the gas status. In the Available Statuses scroll box select the status 1025-FPCpress 1026-FPCFlow and move these parameters to the Selected Statuses scroll box using the >> When the statuses are defined click OK to exit and save. Figure 4.11 The system will at this point read the selected statuses. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-7 Chapter 4 INSTRUMENT PREPARATION Figure 4.12 If the flow and pressure values are correct, click OK to quit this window. If the flow and pressure values are not yet reached wait some more minutes and repeat the operation above. Remark: A 50 litre bottle at 200 bars will last approximately 18 months. Check regularly the gas level of the bottle. To prevent contamination, don’t wait until it gets completely empty before exchanging it. Environment Setting To select the environment, perform the following actions: Click on Tools in the main menu. Click on Action. Click on Set X-Ray Chamber Environment. Select Vacuum. Click on OK. Figure 4.13 4-8 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION Chapter 4 The system will start the pumping process. It is possible to monitor the sequences on the XQIM display. At the end of the process the sample loading system is initialised. The following parameters can be monitored on the ARL Intellipower Series display. PUMPING PC: > 1000 PA → 0 kV 0 m A OFF Figure 4.14 PUMPING SP: > 1000 PA ↓ 0 kV 0 m A OFF Figure 4.15 Sign ↑ ↓ → Description The estimated pressure is increasing The estimated pressure is decreasing The estimated pressure is constant To confirm the vacuum environment is achieved, the ARL 9900 Intellipower Series instrument display must show ‘STAND BY’ in the first display. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-9 Chapter 4 Switch on the XRF X-ray Tube Power Supply Click on Tools in the main menu. Click on Action. Click on Set X-Ray Tube Power. INSTRUMENT PREPARATION Figure 4.16 Select On Slow. Select the kV and mA working condition (30 kV and 80 mA for example). Remark: The condition is depending upon the type of X-Ray tube power supply. Figure 4.17 Click on OK. The system will switch on the generator indicating the start with a buzzer and lighting the X-Ray ON bulbs. The power increase can be monitored on the XSN display. It is recommended to keep the X-ray tube constantly in operation (24/24 hours) in order to avoid thermal stress on the filament. See Eco mode operation to save energy when the instrument is not in use for analysis. 4-10 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION Chapter 4 Switch on the Full XRD X-ray Tube Power Supply (applicable on Workstation only) Click on Tools in the main menu. Click on Monitoring and Troubleshooting. Click on Monitoring Peripheral Devices. Click on ICS. In the dialog box write XR 45,40,4,1,1 Click Send button Figure 4.18 Select the kV and mA working condition. 45 kV and 40 mA for example. Remark: The condition is depending upon the type of X-Ray tube power supply. The system will switch on the generator indicating the start with a buzzer and lighting the X-Ray ON bulbs. The power increase can be monitored on the XSN display. It is recommended to keep the X-ray tube constantly in operation (24/24 hours) in order to avoid thermal stress on the filament. See Eco mode operation to save energy when the instrument is not in use for analysis. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-11 Chapter 4 Eco Mode Setting INSTRUMENT PREPARATION Eco Mode is a mode in which, when the instrument has not been used for a certain length of time, the X-ray power decreases to a pre-defined power. It is also possible to set the firmware in such a way that the power is raised automatically to specific working conditions at a pre-defined hour on specified dates. Eco Mode Setting: Click on Tools in the main menu. Click on Action. Click on Set X-Ray Tube Eco Mode. Figure 4.19 This causes the dialog box shown in the next figure to be displayed. This dialog box is divided into three parts; the upper part allows definition of the conditions during the Eco mode period. The second part allows definition of the exit time when the Eco Mode has to be left and the X-ray power conditions to which the instrument should return. The third part allows the definition of the exit days, months and years the Eco Mode has to be left or days the eco mode should be kept. 4-12 ARL 9900 INTELLIPOWER Series User Manual AA83654 INSTRUMENT PREPARATION Chapter 4 Figure 4.20 Enter Eco Mode Parameters This allows defining the X-ray power conditions during the Eco Mode and how these conditions should be reached. Enabled kV mA This check box has to be checked to allow the modification of the parameters and to activate the Eco Mode. This is the kV value to be reached in Eco Mode (40 kV is recommended). This is the mA value to be reached in Eco Mode (20 mA is recommended). Duration to reach the conditions (Minutes) The value entered here defines the time during which the conditions are continuously changed until the final Eco Mode conditions (kV/mA) are reached. A duration of 60 minutes is the recommended value. Delay (Minutes) The Eco Mode is started after the instrument has been idle for the time specified here. A delay of 60 minutes is the recommended value. AA83654 ARL 9900 INTELLIPOWER Series User Manual 4-13 Chapter 4 Exit Eco Mode Parameters INSTRUMENT PREPARATION This allows defining the dates and hour at which the X-ray power conditions should be raised to a specified setting. Furthermore, the way how these conditions should be reached can also be specified. Enabled kV mA This check box has to be checked to modify the parameters and to cause the settings to be activated. This is the kV value to which the X-ray power setting should return when leaving the Eco Mode. This is the mA value to which the X-ray power setting should return when leaving the Eco Mode. Exit Time (hh:mm) This defines the time of the given dates at which the Eco Mode should be left to reach the working conditions specified hereafter. Duration to reach the conditions (Minutes) This value defines the time during which the X-ray power is continuously raised until the final working conditions (kV/mA) are reached. A duration of 60 minutes is the recommended value. Delay before re-entering Eco Mode (Minutes) This value defines the delay before the instrument should again return to the Eco Mode in case the instrument remained idle over the whole period specified here. A delay of 60 minutes is the recommended value. Select Exit Day(s) If the date specification should be restricted to certain days of the week on which the Eco Mode should not be left (weekends), then these days can be selected here. Exit Every Day This check box allows you either to select the day, the month, and the year of eco mode exit, or to define the days where the eco mode is not exited. If the box is unchecked the exit days month and year are accessible to be defined. In that case the No Exit Days List box is disabled. To the other hand if the box is checked, the day, month, year box is disabled and the No Exit Days List box is enabled, thus allowing the definition of the days where the Eco Mode should not be quit. No Exit Day List This box allows the definition of the days where the Eco Mode should not be quit. If no day, in the No Exit Days List should be selected click on “…” at bottom of the list box. After each modification of one of the parameters described above, the dialog box has to be left by clicking onto the OK button to store the new values. Instrument technical data For the instrument technical data, laboratory conditions and safety standards please refer to the ARL Intellipower Series Pre-installation Manual. ARL part number AA83656. 4-14 ARL 9900 INTELLIPOWER Series User Manual AA83654 5 SAMPLE PREPARATION SAMPLE PREPARATION Chapter 5 5 SAMPLE PREPARATION Since X-ray spectrometry is essentially a comparative method of analysis, it is vital that all standards and unknown samples are presented to the spectrometer in a reproducible and identical manner. The quality of sample preparation in X-ray fluorescence analysis is as important as the quality of measurements. The preparation method: ♦ Must give specimen with similar physical properties, including mass absorption coefficient, density and particle size, for a certain calibration range; ♦ Must not introduce extra significant systematic errors, for example, the introduction of trace elements from contaminants in a diluents; ♦ Must be rapid and cheap. Note: For quantitative analysis, samples must be prepared in the same way like the standard samples used for calibration. An adequately prepared sample: ♦ Must be representative of the material; ♦ Must be homogeneous; ♦ Must, when possible, be thick enough to meet the requirements of an infinitely thick sample. Various preparation techniques have been described in the literature. The object of this chapter is to point out the main criteria for quality preparation of solid, metallic samples, powder samples, and liquid samples. The following table shows typical methods of sample preparation. Type Sample Iron Steel Nickel Ferro-Alloy Cu-alloy Al-alloy Pb-alloy Zn-alloy Metallic Chemicals Polymer Plant Ceramic Ore Soil Sediment Oxide Cutting Preparation Surface grinding with belt surfacer Purpose Surface smoothing Sample holder Standard cassette Solid Cutting Surface milling with lathe Surface smoothing Standard Cassette Grinding Briquetting Equalizing the density and surface smoothness Eliminating the mineralogical and the granulometric differences Standard Cassette Powder Grinding Fusion Standard Cassette AA83654 ARL 9900 INTELLIPOWER Series User Manual 5-1 Chapter 5 SAMPLE PREPARATION Sample Preparation for Solids The purpose of preparation is smoothing the surface of the sample. For most analyses, scratch-free surfacing is necessary. For the analysis of light elements, even mirror-like surfaces are often required. For this aim, two polishing methods are applied: Surface Milling and Lathe: for soft metals; Surface Grinding: for hard alloys and brittle materials such as ceramics. The difficulty with surface finish is polishing striation. It gives rise to the so-called shielding effect, which results in the decrease of fluorescence intensities. As expected the decrease in intensity is more important for lighter elements when the primary radiation are perpendicular to the striations and weaker when they are parallel to them. For that reason, modern spectrometers are equipped with spinning sample holders to smooth out the influence of sample orientation, resulting in observed intensities on samples and standards that are reproducible. However, the shielding effect may still be present; sample rotation will compensate for it only if the magnitude of the effect is the same for standards and production samples; this requires that the striation be of the same size and that the sample composition be similar (same effective wavelength). In the following, we will give some general remarks on the preparation of hard and soft metals. Soft metals (for example Al, Cu, Mg, Zn or Sn bases) Striations deeper than few µm may impair significantly the accuracy of determinations. Furthermore, there is a risk of smearing of the softer components: the intensities of the elements in softer phases increase while those of the harder phases decrease. To obtain the desired surface finish, special precautions must be taken even during milling and especially in the final polishing operation. Hard metals (for example Fe, Ni, Co bases) Striation depths of 100 µm are acceptable for elements with characteristic lines of short wavelengths. To obtain the desired surface finish, fine grits of Al2O3, SiC, B4C (80-180 grits) have to be used. However, polishing may be source of contamination, since currently used abrasives, SiC and Al2O3, contain two elements that are often determined in commercial alloys. In this case, it may be necessary to clean the sample surface to remove these contaminations as well as grease stains and handling residuals. 5-2 ARL 9900 INTELLIPOWER Series User Manual AA83654 SAMPLE PREPARATION Chapter 5 Shape Cut to required size: Casting method Melt 52 mm diam. max. 30 mm height max. Cast Mold Base Cool rapidly Surface Grinding Abrasive paper Grinding stone Steels, Co, Ni, etc. Cast iron, hard metal Milling or lathe Soft metals, (Al, Cu, Mg, etc To cassette or sample stage Figure 5.1 AA83654 ARL 9900 INTELLIPOWER Series User Manual 5-3 Chapter 5 SAMPLE PREPARATION Sample Preparation for Powders The analysis of powder is invariably more complex than that of metallic sample. In addition to interelement interferences and macro scale heterogeneity, particle size effects and mineralogical effects are also important. Although inhomogeneity and particle size can often be minimized by grinding below 50 microns and pelletizing at high pressure, often the effects cannot be completely removed because the harder compounds present in a particular matrix are not broken down. These effects produce systematic errors in the analysis of specific type of material e.g. siliceous compounds in slags, sinters and certain minerals. Two methods of sample preparation for powders are explained in the following: Briquet method Fusion technique Briquet method The quickest and simplest method of preparation is to press them directly into briquets (or pellets) of constant density. This method can be applied where powders are not affected by particle size limitations. If the self-bonding properties of the powder are good and provided that the powder particles are less than about 50 microns in diameter the sample will pelletize at around 10-30 tons. Where the self-bonding properties of the powder are poor, higher pressure may have to be employed or in extreme cases a binder will be added before pelletizing. The binding agent must be chosen with care. It must have the following properties: Good self-bonding properties Be free from significant contaminant elements Have low absorption. Be stable under vacuum and irradiation conditions Must not introduce significant interelement interferences. Of the large number of binding agents, which have been successfully employed probably the most useful are wax and methylcellulose. Crush, grind and mix To grain size 10 %) Minor (0.5 - 10 %) Traces (