S8 TIGER Operators Manual DOC-M80-EXX032 V3 Complete

XRFthink forward

Bruker AXS GmbH

S8 TIGER

Operator's Manual

The reproduction, transmission or use of this document or its contents is not permitted without express written authority. Offenders will be liable for damages. All rights reserved.

We have checked the contents of this manual for agreement with the hardware and software described. Since deviations cannot be precluded entirely, we cannot guarantee full agreement. However, the data in this manual are reviewed regularly and any necessary corrections are included in subsequent editions. Suggestions for improvement are welcome.

All configurations and specifications are subject to change without notice.

Order no. DOC-M80-EXX032 V3. Updated: November 30, 2009.

2007 - 2009 Bruker AXS GmbH, Karlsruhe, Germany.

All trademarks and registered trademarks are the sole property of their respective owners.

Printed in the Federal Republic of Germany.

Bruker AXS GmbHstliche Rheinbrckenstr. 4976187 Karlsruhe, GermanyTel. +49 (7 21) 5 95-28 88Fax +49 (7 21) 5 95-45 [email protected]

S8 TIGER X-Ray Spectrometer

Operators Manual

Contents S8 TIGER Operators Manual

DOC-M80-EXX032 V3 11. 2009

DOC-M80-EXX032 V3 11. 2009 i

S8 TIGER X-ray Spectrometer Table of Contents

1 Safety Guidelines .............................................................................................1-1 Warning Symbols........................................................................................................................ 1-1 Qualified Personnel .................................................................................................................... 1-3 Correct Usage.............................................................................................................................. 1-3 General Safety Precautions of the S8 TIGER........................................................................... 1-5 Biological Effects ...................................................................................................................... 1-12

Mechanisms of Damage ...................................................................................................... 1-12 Tissue Sensitivity ................................................................................................................. 1-12 Prompt and Delayed Effects ................................................................................................ 1-13 Delayed Effects of Radiation Exposure ............................................................................... 1-14

2 General Physical Principles ............................................................................2-1 Production of X-rays................................................................................................................... 2-1

Continuous Spectrum ............................................................................................................ 2-2 Characteristic Spectrum......................................................................................................... 2-3

The Bragg Equation .................................................................................................................... 2-6 Scintillation counter.................................................................................................................... 2-8 Proportional counter................................................................................................................... 2-8


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3 Introduction to the Instrument........................................................................ 3-1 Overview of this Manual ............................................................................................................. 3-1 Overview of the Product ............................................................................................................. 3-2 Overview of the Operation Principle ......................................................................................... 3-3 Instrument Components............................................................................................................. 3-8

Illuminated Status Display.................................................................................................... 3-15 LED Guide..................................................................................................................... 3-15

Measurement Execution Basics of the S8 TIGER.................................................................. 3-16 Flow Chart Showing Standard Operation............................................................................. 3-19

Network Configuration.............................................................................................................. 3-21 Use of an External PC.......................................................................................................... 3-22

4 Switching the Instrument On and Off............................................................. 4-1 Switching On Auto Start Up of the S8 TIGER........................................................................ 4-1 Switching Off Power-off Procedure........................................................................................ 4-6

Switching Off Using TouchControlTM...................................................................................... 4-6 Switching Off Without UsingTouchControlTM.......................................................................... 4-8

5 TouchControl Operation.............................................................................. 5-1 5.1 Introduction ................................................................................................................... 5-1 5.2 TouchControl User Interface.................................................................................... 5-1

5.2.1 TouchControl Controls ......................................................................................... 5-2 5.2.2 Logging into TouchControl ................................................................................... 5-6 5.2.3 TouchControl Main Screens................................................................................. 5-8 5.2.4 Loader Screen ......................................................................................................... 5-8 5.2.5 Results Screen....................................................................................................... 5-10 5.2.6 Status Screen ........................................................................................................ 5-11 5.2.7 Tools Screen.......................................................................................................... 5-12

5.3 Results Database ........................................................................................................ 5-13 5.3.1 Advanced Search................................................................................................... 5-14

S8 TIGER Operators Manual Contents

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5.3.2 Sorting and Printing Results .................................................................................. 5-15 5.3.2 Invalidating Results................................................................................................ 5-15

5.4 Status ........................................................................................................................... 5-16 5.4.1 Schedule................................................................................................................ 5-18

5.5 Tools ............................................................................................................................ 5-19 5.5.1 Appearance ........................................................................................................... 5-19 5.5.2 Measure................................................................................................................. 5-20 5.5.3 Options .................................................................................................................. 5-21 5.5.4 User Editor............................................................................................................. 5-23 5.5.5 S8Tools.................................................................................................................. 5-26 5.5.6 Help & About.......................................................................................................... 5-28

5.6 Alarms.......................................................................................................................... 5-29

6 Operating the S8 TIGER...................................................................................6-1 Measuring Samples with QUANT-EXPRESS............................................................................ 6-1

Sample Preparation ............................................................................................................... 6-2 Basic Operation without Touchscreen ..................................................................................... 6-3 Basic Operation with TouchControlTM ...................................................................................... 6-3

Routine Check........................................................................................................................ 6-3 Instrument Performance Verification S8 CHECK ........................................................ 6-4 Verification of the Installation of QUANT-EXPRESS QE CHECK............................... 6-6

Performing a Measurement with QUANT-EXPRESS............................................................ 6-9 Step 1: Sample I.D........................................................................................................ 6-10 Step 2: Material............................................................................................................. 6-12 Step 3: Preparation....................................................................................................... 6-14 Step 4: Mode................................................................................................................. 6-16 Step 5: Diameter ........................................................................................................... 6-18 Step 6: Measurement Method ...................................................................................... 6-20 Starting the Measurement ............................................................................................ 6-22 Viewing and Printing the Results .................................................................................. 6-24

User Calibrations with SPECTRAplus ....................................................................................... 6-26


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7 Servicing and Maintaining the Spectrometer System .................................. 7-1 Cleaning the Spectrometer System........................................................................................... 7-1 Handling the STG Samples ........................................................................................................ 7-2 Refilling the Deionized Water of the Internal Cooling Unit ..................................................... 7-3

Important Safety Instructions ................................................................................................. 7-3 How to Check the Water Level?............................................................................................. 7-5 Refilling the Cooling Water..................................................................................................... 7-7

Changing the P10 Detector Gas............................................................................................... 7-12 Reason ................................................................................................................................. 7-12 Changing the Tank ............................................................................................................... 7-12 Checking the HV-Alignment ................................................................................................. 7-20

S8 TIGER...................................................................................................................... 7-20 Checking User Specific Calibrations .................................................................................... 7-22 Checking the S8 TIGER and QUANT-EXPRESS with S8 CHECK and QE CHECK .......... 7-23 Recalibration- Drift Correction.............................................................................................. 7-25

Consumables ............................................................................................................................. 7-26 Maintenance Parts Package S8 TIGER Order Number A15D103/A15D113..................... 7-26

Time Intervals for Preventive Maintenance.......................................................................... 7-27 Service Contracts ...................................................................................................................... 7-27

8 Troubleshooting the System........................................................................... 8-1 1. Using the First Aid Button on the Touchscreen .................................................................. 8-1 2. Calling the Bruker AXS Hotline.............................................................................................. 8-3

2.1 Participating in a WebEx Session .................................................................................... 8-3 Connecting to WebEx ..................................................................................................... 8-3 Joining a WebEx Session ............................................................................................... 8-6 Desktop Sharing and File Transfers ............................................................................. 8-11 Leaving the Session...................................................................................................... 8-12

2.2 Using Spectra Mail ......................................................................................................... 8-13 Aim ................................................................................................................................ 8-13 Starting Spectra Mail..................................................................................................... 8-13 Creating a Spectra Mail File.......................................................................................... 8-13


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Reference: List of Menus in Spectra Mail ..................................................................... 8-16 3. Trouble Shooting Flowchart ................................................................................................ 8-17

9 Overview S8 TIGER Solutions.........................................................................9-1 PETRO-QUANT Version 2.0 or Higher ...................................................................................... 9-1

PETRO-QUANT BASIC for the S8 TIGER The XRF Solution for the Petrochemical Industry.................................................................. 9-1

GEO-QUANT Version 1.3.1 or Higher........................................................................................ 9-3 GEO-QUANT for the S8 TIGER Advanced Geological Trace Element Analysis by XRF .. 9-3

CEMENT-QUANT ......................................................................................................................... 9-5 CEMENT-QUANT for the S8 TIGER The XRF Solution for the Cement Industry.............. 9-5

MLplus ............................................................................................................................................ 9-7 MLplus Multilayer and Thin Film Software ............................................................................... 9-7

QUANT-EXPRESS ....................................................................................................................... 9-8 Standardless Analysis Package............................................................................................. 9-8

10 S8 TIGER Parts ...............................................................................................10-1 Spare Parts Packages S8 TIGER ............................................................................................. 10-1

Basic Spare Parts Package for S8 TIGER 1kW Order Number A15D100.......................... 10-1 Basic Spare Parts Package for S8 TIGER 3/4kW Order Number A15D110....................... 10-4 Extension Spare Parts Package S8 TIGER 3/4kW Order Number A15D111 ..................... 10-7

Optional Parts S8 TIGER .......................................................................................................... 10-8 Sample Holders.................................................................................................................... 10-8 Sample Holder Masks and Accessories .............................................................................. 10-9 Collimators, Masks and Crystals........................................................................................ 10-11 Accessories for Liquid Samples......................................................................................... 10-12 Reference, Calibration and Samples ................................................................................. 10-14 Spare Parts, Application Support, Training Courses ......................................................... 10-14


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11 S8 TIGER Specifications ............................................................................... 11-1 Analytical Performance ............................................................................................................ 11-1 Instrument Specification .......................................................................................................... 11-2 Certified Compliance................................................................................................................. 11-5 Electrical Specification ............................................................................................................. 11-6

High-voltage Generator................................................................................................. 11-7 X-ray Tubes ................................................................................................................................ 11-8 Laboratory Requirements......................................................................................................... 11-9

S8 TIGER Mechanical Specifications .................................................................................. 11-9 Environmental Specifications ............................................................................................... 11-9 Gas Consumption............................................................................................................... 11-10

Helium/Nitrogen Operation ......................................................................................... 11-10 Accessories ............................................................................................................................. 11-10

UPS for the S8 TIGER ....................................................................................................... 11-11 Water Chiller for the S8 TIGER (3kW or 4kW only) ........................................................... 11-13

12 References ..................................................................................................... 12-1 List of Available XRF and S8 Documentation ........................................................................ 12-1

13 Index ............................................................................................................... 13-1

14 Fold-out Periodic Table ................................................................................. 14-1


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Figures Fig. 2-1: Schematic diagram of an X-ray tube. ................................................................................................ 2-1 Fig. 2-2: Production of continuous (white) radiation. ....................................................................................... 2-2 Fig. 2-3: Production of characteristic radiation simplified representation...................................................... 2-3 Fig. 2-4: Subshells and their transferred electrons. ......................................................................................... 2-4 Fig. 2-5: Spectrum of an X-ray tube. ............................................................................................................... 2-5 Fig. 2-6: Fulfillment of the Bragg equation....................................................................................................... 2-6 Fig. 3-1: S8 TIGER with EasyLoad and TouchControl............................................................................... 3-4 Fig. 3-2: X-ray beam path of the S8 TIGER. ................................................................................................... 3-5 Fig. 3-3: Overview of the typical elemental range for the three standard analyzer crystals. For a more

detailed periodic table, please, consult the appendix. ....................................................................... 3-6 Fig. 3-4: Front view of the S8 TIGER. ............................................................................................................. 3-9 Fig. 3-5: Inside the loader (sample magazine). ............................................................................................. 3-10 Fig. 3-6: View on the instrument after removing the front and the right side panel with several

components labelled. ...................................................................................................................... 3-11 Fig. 3-7: View on the instrument after removing the front and the left side panel with several

components labelled. ...................................................................................................................... 3-12 Fig. 3-8: View on the 3 or 4kW version after removing the back and the left (viewed from front) side

panel with several components labelled.......................................................................................... 3-13 Fig. 3-9: View on the 3 or 4 kW version after removing the back and the right (viewed from front) side

panel with several components labelled.......................................................................................... 3-14 Fig. 3-10: Status display.................................................................................................................................. 3-15 Fig. 3-11: Flow chart showing standard operation........................................................................................... 3-20 Fig. 3-12: S8 TIGER SPECTRAplus PC network connection. ........................................................................ 3-21 Fig. 4-1: Settings in System Configuration for the auto start up procedure. .................................................... 4-2 Fig. 4-2: Control panel..................................................................................................................................... 4-3 Fig. 4-3: Status display.................................................................................................................................... 4-3 Fig. 4-4: Login screen of S8 TouchControl (see Step 12) ............................................................................... 4-5 Fig. 4-5: Shutdown. ......................................................................................................................................... 4-7 Fig. 4-6: Confirm the shutdown. ...................................................................................................................... 4-7 Fig. 4-7: S8 Tools Connect button................................................................................................................... 4-8


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Fig. 4-8: Control panel .....................................................................................................................................4-9 Fig. 5-1: To log-in to the S8 TIGER you will need to enter your username and password ..............................5-7 Fig. 5-2: The Loader screen will display the Application Chooser when an empty position is selected on

the Sample Magazine........................................................................................................................5-9 Fig. 5-3: The Results screen allows access to all stored results on the S8 TIGER. ......................................5-10 Fig. 5-4: The Status screen displays the current status of the machine. .......................................................5-11 Fig. 5-5: The Tools screen contains pages to change settings and information. ...........................................5-12 Fig. 5-6: Completed samples show results which can be printed. .................................................................5-13 Fig. 5-7: Advanced Search options................................................................................................................5-14 Fig. 5-8: Search Options................................................................................................................................5-15 Fig. 5-9: A confirmation is required to invalidate a sample. ...........................................................................5-16 Fig. 5-10: The Status screen shows the current status of the machine. ..........................................................5-17 Fig. 5-11: The Schedule page shows are samples in the measurement queue. .............................................5-18 Fig. 5-12: The Appearance page contains options that affect the appearance of the Loader screen. .............5-19 Fig. 5-13: The Measure page contains options that affect the measurement. .................................................5-20 Fig. 5-14: The Options page contains options that affect the settings. ............................................................5-21 Fig. 5-15: Add an application to the Shortcuts .................................................................................................5-22 Fig. 5-16: The User editor page is used to add a new user or change the privileges of an existing user. .......5-23 Fig. 5-17: Adding a new user...........................................................................................................................5-24 Fig. 5-18: Users can have various privileges which are shown above.............................................................5-25 Fig. 5-19: S8Tools allow the operator to insert a manual mask and diagnose.................................................5-26 Fig. 5-20: Mask change. Simply select the required mask change above. ......................................................5-27 Fig. 5-21: The About page contains version information and contact details...................................................5-28 Fig. 5-22: An Alarm message. In this example a generator error is reported. .................................................5-29 Fig. 6-1: Loader screen S8 CHECK.................................................................................................................6-4 Fig. 6-2: Results check for the instrument performance verification S8 CHECK. ............................................6-5 Fig. 6-3: Loader screen QE CHECK................................................................................................................6-7 Fig. 6-4: Results check for the QE CHECK measurement...............................................................................6-8 Fig. 6-5: Loader screen select QUANT-EXPRESS........................................................................................6-10 Fig. 6-6: Enter sample ID...............................................................................................................................6-11 Fig. 6-7: Sample materials.............................................................................................................................6-13 Fig. 6-8: Selection of the sample preparation. ...............................................................................................6-15


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Fig. 6-9: Selection of the measurement mode............................................................................................... 6-17 Fig. 6-10: Selection of the sample mask diameter........................................................................................... 6-19 Fig. 6-11: Selection of the measurement method............................................................................................ 6-21 Fig. 6-12: Start the measurement.................................................................................................................... 6-22 Fig. 6-13: Status during the measurement. ..................................................................................................... 6-23 Fig. 6-14: Results after the measurement. ...................................................................................................... 6-24 Fig. 6-15: Result screen. ................................................................................................................................. 6-25 Fig. 7-1: S8 Tools instrument warning Cooling water level. .......................................................................... 7-6 Fig. 7-2: Disconnect the mains power. ............................................................................................................ 7-7 Fig. 7-3: Backside view. .................................................................................................................................. 7-8 Fig. 7-4: Backside view with removed back panel. .......................................................................................... 7-9 Fig. 7-5: Refill of the deionized water reservoir. ............................................................................................ 7-10 Fig. 7-6: Reconnect to the mains power........................................................................................................ 7-11 Fig. 7-7: S8 TOOLS ONLINE Counter Gas. ............................................................................................ 7-13 Fig. 7-8: S8 TOOLS ONLINE Counter Gas Off. ...................................................................................... 7-14 Fig. 7-9: S8 TOOLS ONLINE Counter Gas Status. ................................................................................. 7-15 Fig. 7-10: S8 TOOLS ONLINE Counter Gas On. ...................................................................................... 7-17 Fig. 7-11: S8 TOOLS ONLINE Counter Gas Set flag. ............................................................................... 7-18 Fig. 7-12: SpectrometerAlignment................................................................................................................... 7-19 Fig. 7-13: Loader Drift correction S8 CHECK and QE CHECK. ................................................................ 7-24 Fig. 8-1: S8Tools screen with the first aid button............................................................................................. 8-2 Fig. 8-2: Invitation to support session email .................................................................................................... 8-4 Fig. 8-3: Web site Support Session page ........................................................................................................ 8-5 Fig. 8-4: WebEx Pre-Session Form................................................................................................................. 8-6 Fig. 8-5: Install WebEx Client ActiveX control ............................................................................................... 8-8 Fig. 8-6: Security Warning window.................................................................................................................. 8-9 Fig. 8-7: Welcome to Support Center window............................................................................................. 8-10 Fig. 8-8: Allow Desktop Control and/or File Transfers dialogs....................................................................... 8-11 Fig. 8-9: Desktop sharing .............................................................................................................................. 8-12 Fig. 8-10: Spectra Mail options menu.............................................................................................................. 8-15 Fig. 8-11: Trouble shooting flowchart. ............................................................................................................. 8-18


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Tables Tab. 3-1: LED guide........................................................................................................................................3-15 Tab. 3-2: Overview of the S8 TIGER atmospheric measurement modus. Please note that some modes

are optional......................................................................................................................................3-17 Tab. 6-1: Sample preparation techniques for typical samples ..........................................................................6-2 Tab. 6-2: Evaluation models of QUANT-EXPRESS........................................................................................6-12 Tab. 6-3: QUANT-EXPRESS measurement methods ....................................................................................6-20 Tab. 6-4: Files needed for SPECTRAplus custom calibrations. ........................................................................6-26 Tab. 7-1: List of consumables.........................................................................................................................7-26 Tab. 7-2: Package A15D103/A15D113 content ..............................................................................................7-26 Tab. 8-1: List of menus in Spectra Mail. .........................................................................................................8-16 Tab. 11-1: Instrument specification...................................................................................................................11-2 Tab. 11-2: Certified compliance ........................................................................................................................11-5 Tab. 11-3: Electrical specification .....................................................................................................................11-6 Tab. 11-4: Electrical Specification continued ....................................................................................................11-7 Tab. 11-5: Recommended X-ray tubes.............................................................................................................11-8 Tab. 11-6: S8 TIGER system dimensions and weight ......................................................................................11-9 Tab. 11-7: Environmental specifications ...........................................................................................................11-9 Tab. 11-8: Gas specifications .........................................................................................................................11-10 Tab. 11-9: UPS TYPE Effekta Pegasus 31 (1 ph.) .........................................................................................11-11 Tab. 11-10: UPS TYPE Toshiba 1600EP (1 ph.) ..............................................................................................11-11 Tab. 11-11: UPS TYPE Effekta Pegasus 31 (1 ph.) .........................................................................................11-12 Tab. 11-12: UPS TYPE Toshiba .......................................................................................................................11-12 Tab. 11-13: Water chiller ..................................................................................................................................11-13 Tab.12-1: List of Available XRF and S8 Documentation..................................................................................12-1

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1 Safety Guidelines Caution!

To prevent accidents and system damage, read these instructions before installation or use. Only operate the S8 TIGER after you have understood and followed the safety warnings and instructions!

Warning Symbols All of the following symbols (except the Biohazard Warning) are displayed on the S8 TIGER system. Strictly obey all instructions and the warning text printed on the labels attached to the parts of the equipment.

Radiation Danger!

Risk of Electric Shock!

Caution! Read the Operating Instructions!

Safety Guidelines S8 TIGER Operators Manual

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Danger of Injury! Danger of Crushing!

Warning: Hot Surfaces!

Danger of Toxic Substances!

General Biohazard Warning!

Follow all valid national, state, and local regulations for disposal.

Protective Ground/Earth Terminal

S8 TIGER Operators Manual Safety Guidelines

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Qualified Personnel Danger: Potentially toxic or hazardous samples!

To prevent any risk for health and safety the analysis of samples with the S8 TIGER, in-cluding handling and/or preparation steps, must be entrusted only to persons who have qualifications in accordance with their activities and functions and who, based on their technical training, their knowledge and experience and their knowledge of the applicable standards, are able to evaluate the work assigned to them and recognize possible haz-ards. This also includes the knowledge of applicable accident prevention regulations, gen-erally recognized safety regulations, EC guidelines and country-specific standards and regulations. Carefully read and follow all safety and handling advice in the appropri-ate material safety data sheets.

The S8 TIGER spectrometer system or its parts may only be set up and operated in conjunction with this manual. Only qualified personnel may be allowed to work on this equipment.

The installation, maintenance and repair of the spectrometry system may be carried out only by per-sonnel who are authorized by Bruker AXS.

All repairs, adjustments and alignments performed on any components of the S8 TIGER system (in-cluding the host computer) must be carried out in strict accordance with the established safety prac-tices and standards of the country in which the equipment is installed.

Correct Usage The instrument was designed to perform element analysis by means of X-ray fluorescence. This de-vice and its components may only be used for the applications described in the technical description or in the Bruker AXS literature (e.g. XRF Lab Reports or XRF Application Reports). You can request those reports from your local Bruker AXS Service or Sales Representative. It may only be used in connection with devices or components from other manufacturers that have been approved or recom-mended by Bruker AXS, for example for automation solutions.


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Warning!

This product can only function correctly and safely if it is transported, stored, set up, and installed correctly, and if it is operated and maintained as recommended by Bruker AXS. Disclaimer and Liability Bruker AXS has checked the contents of this manual for agreement with the hardware, firmware, and software described. Since deviations cannot be excluded entirely, Bruker AXS cannot guarantee full agreement. However, the information in this manual is reviewed regularly and any necessary correc-tions are included in subsequent editions. Suggestions for improvements are welcome. Send them to [email protected].


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General Safety Precautions of the S8 TIGER Danger: X-ray Radiation!

The S8 TIGER spectrometer system is an analytical instrument with a strong X-ray source. Shielding and safety equipment guarantee that the emitted radiation does not exceed 1.0 Sv/h during operation. Shielding and safety features designed into the equipment guarantee that the emitted radiation does not exceed 1.0 Sv/h (at 5 cm from any external surface of the device) during operation. This level is below the regulatory limit in all jurisdictions. The ICRP dose limits in Publication 60 and 103 to the whole body for a radiation worker averaged over a 5-yr period is 20 mSv in a year, and for a member of the public it is 1 mSv in a year. It is highly unlikely that the radiation worker dose limits will be exceeded when trained and qualified personnel use such devices. Read the section Protection Against Radiation of the S8 TIGER Introductory User Manual (order number DOC-M80-ZXX031) before turning on the system. Please observe local regulations for the operation of X-ray systems. If you suspect that the safety system does not work correctly or that radiation protection is impaired for any reason, immediately switch off the system and contact your local Bruker AXS Service Representative. Manipulations and modifications of the safety systems are strictly forbidden!

Note

The X-ray generator is controlled by a three position Keyed switch (OFF/NEUTRAL/ON) similar to the ignition switch of a car. The key can only be removed when the switch is in the OFF position. The switch will remain in the OFF position until the key is inserted and turned. Therefore the removal of the key will terminate production of X-ray.


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Warning: High-Voltage!

Inside the S8 TIGER, voltages up to 60 kVDC occur which are however not accessible from the outside. High voltages exist in the high-voltage generator and X-ray tube, as well as in the connecting high-voltage cable. In addition, the radiation detectors are operated with high voltages up to 2.3 kVDC. If one of these high-voltage components is damaged, switch off the system immediately and contact your local Bruker AXS Service Representative.

Warning: Danger of Voltage!

The system must be operated ONLY with such mains supply voltages as are listed on the spectrometers rear plate. As long as the system is connected to the external mains sup-ply, some terminals of the internal components may present a danger of high-voltage shock.

Warning: Electrical Hazards due to Leakage of Cooling Water!

Inside the S8 spectrometer there are closed loop water circuitries for cooling the X-ray tube, the X-ray generator and also for the internal air-conditioning. In addition to that, S8-3kW and S8-4kW instruments are provided with water hoses which are connected to the buildings water supply system. If there are any water leakages (caused by faulty components or by accident during the refilling of the internal water reservoir) the S8 spectrometer must remain switched off or be turned off instantly! This must be done by switching off the automatic circuit breaker or power disconnector which is located in the vicinity of the instrument. It is not sufficient to just turn off the spectrometer using the power-off button as some terminals inside the instrument will stay connected to mains supply voltage. The S8 must stay powered-off until the leakage source has been repaired and all wet re-gions have been dried thoroughly. Be aware, there is a high danger of electrical shocks whenever there is leakage of water!


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Warning: Danger due to Moving Parts and Components!

While the instrument is running there is an enhanced risk of injuries due to moving parts and components. It is the responsibility of the operator to assure that no person can touch or get close to the following components or units while the instrument is running: - Sample turn unit (e.g., for automation systems) If in doubt, if the instrument is already running, stay away from its components! Do not check motion by using your hand!

Caution: Moving Mechanical Components!

The samples to be measured are positioned by means of a fast XYZ sample changer sys-tem. To prevent personal injury, all motions are immediately stopped if the sample maga-zine cover is opened. If you suspect that the safety system does not work correctly, immediately switch off the system and contact your local Bruker AXS Service Representative. Manipulations and modifications of the cover control are strictly forbidden!

Warning: Change of the Instruments Location!

The S8 TIGER spectrometer is designed to be a mobile analytical instrument. During transportation, please avoid mechanical shocks to avoid damaging the sensitive physical components. After each change of location, the S8 TIGER must be checked by staff authorized and trained by Bruker AXS! Please contact your Bruker AXS Service Representative.


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Warning: Hot Surfaces!

Several components (mainly all stepper motors, the air heating element, the water pump and the vacuum pump) of the S8 spectrometer get very hot during standard operation due to power dissipation and could cause severe burns when being touched. Normally, these components cannot be accessed as the S8s side panels are installed and, the motors inside the sample loader are covered by metal pieces. But, during maintenance and repair the hot surfaces could be touched by accident. Be aware that the surface temperature of internal S8 components might exceed 100C (212F) whenever the S8 is switched on. Before touching any of these components turn off the instrument and wait until the components have cooled down sufficiently.

Caution: Oil!

The vacuum pump uses oil as a lubricant. Disposal of oil must comply with all applicable national, state, and local regulations.

Caution: Batteries!

Some circuit boards inside the S8 TIGER are equipped with batteries. Disposal of batter-ies must comply with all applicable national, state, and local regulations.


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Warning: Beryllium!

Do not touch the X-ray tubes radiation outlet window or scintillation detectors front win-dows, as these windows contain beryllium. In case of an implosion of the X-ray tube, you could get hurt by beryllium fragments. This is why you should wear safety goggles and gloves when cleaning the sample chamber or handling the X-ray tube. Fumes or dust from Beryllium and its compounds can be hazardous if inhaled! Corrosion of the beryllium may occur during use. Beryllium must not be cut, machined, or handled in any way. Disposal of beryllium must comply with all applicable national, state, and local regulations.

Warning: Analyzing Toxic Substances!

When analyzing toxic substances, strictly follow national, state, and local safety regula-tions! Only use sample holders recommended by Bruker AXS for the respective measurements.

Warning: Analyzing Biological Active Substances!

When analyzing biologically active substances, follow applicable national, state, and local safety regulations, along with IEC 61010-2-081.


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Warning: Thallium!

The analyzer crystal TLAP contains thallium, an extremely toxic heavy metal. This crystal is water-soluble and can cause poisoning by skin contact. Please handle this crystal with maximum care and avoid any skin contact! Strictly obey the applicable national, state, and local safety regulations. Disposal of thallium-containing parts must comply with all applicable national, state, and local regulations.

Warning: Analyzing Harmful Volatile Substances!

When analyzing harmful volatile substances, strictly follow national, state and local safety regulations! Only use the sample holders recommended by Bruker AXS for the respective measure-ments. A vent to open air should be provided for the exhaust gases of the vacuum pump.

Warning: Gas Operation (P-10, Helium or Nitrogen)!

Systems with gas flow devices require external gas cylinders, if no in-house gas supply system is available. The cylinders must be secured so that the cylinders are prevented from falling over. Correct and secure installation of gas cylinders must be provided at all times! Follow applicable national, state, and local regulations for installation and operation of P-10 (argon-methane gas mixture), helium, and nitrogen gas operation and gas cylinders. A separate vent to open air should be provided to let off the P-10 gas.


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Warning: Inadvertent Use of Wrong Gas Type!

It is the responsibility of the user to assure that the correct gas type is connected to the instrument. Before opening the gas valves leading to the instrument, double check that the desired gas is used. In particular exclude the inadvertent use of any explosive or corrosive gas.

Warning: Disposal of Instrument!

Follow all valid national, state, and local regulations for disposal and contact Bruker AXS Service for additional assistance. The S8 TIGER contains thallium (if the optional TLAP analyzer crystal is installed), beryl-lium (X-ray tube and detector), and batteries (some circuit boards).


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Biological Effects (from Princeton University web page)

Mechanisms of Damage Injury to living tissue results from the transfer of energy to atoms and molecules in the cellular struc-ture. Ionizing radiation causes atoms and molecules to become ionized or excited. These excitations and ionizations can:

Produce free radicals. Break chemical bonds. Produce new chemical bonds and cross-linkage between macromolecules. Damage molecules that regulate vital cell processes (e.g. DNA, RNA, proteins). The cell can repair certain levels of cell damage. At low doses, such as that received every day from background radiation, cellular damage is rapidly repaired.

At higher levels, cell death results. At extremely high doses, cells cannot be replaced quickly enough, and tissues fail to function.

Tissue Sensitivity In general, the radiation sensitivity of a tissue is:

proportional to the rate of proliferation of its cells inversely proportional to the degree of cell differentiation


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For example, the following tissues and organs are listed from most radiosensitive to least radiosensitive:

Most Sensitive: Blood-forming organs Reproductive organs Skin Bone and teeth Muscle Least sensitive: Nervous system

This also means that a developing embryo is most sensitive to radiation during the early stages of differentiation, and an embryo/fetus is more sensitive to radiation exposure in the first trimester than in later trimesters.

Prompt and Delayed Effects Radiation effects can be categorized by when they appear.

Prompt effects: effects, including radiation sickness and radiation burns, seen immediately after

large doses of radiation delivered over short periods of time.

Delayed effects: effects such as cancer induction that may appear months or years after a radia-tion exposure


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Delayed Effects of Radiation Exposure Cancer

Studies of people exposed to high doses of radiation have shown that there is a risk of cancer induc-tion associated with high doses.

The specific types of cancers associated with radiation exposure include leukemia, multiple mye-loma, breast cancer, lung cancer, and skin cancer.

Radiation-induced cancers may take 10 - 15 years or more to appear. There may be a risk of cancer at low doses as well.

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2 General Physical Principles Production of X-rays X-rays are photons that are emitted when electrons strike a metal target and interact with the electrons orbiting the nuclei of the metal atoms. The electromagnetic waves in the -range 0.1 - 2 are emitted in all directions. In X-ray tubes, electrons are emitted by a heated cathode, accelerated, and strike an anode material. The cathode consists of a tungsten filament. For the generation of X-rays, high voltages of 20-60 kV are required. Much of the energy supplied to the tube is transferred to heat, while less than 1% of it is converted into X-rays. The anode consists of a metal (for example, Rh, Mo or Cr) that produces a characteristic wavelength. A water cooling system prevents it from overheating. X-ray tubes usually have a thin Beryllium windows by which the X-rays escape to the outside. The tube is partly clad with a heavy absorbing material such as lead to prevent the X-rays emitted in other directions from penetrating to the outside.

Fig. 2-1: Schematic diagram of an X-ray tube.

Cathode (ring, tungsten filament) Electron beam

X-ray beam

Beryllium window e.g. 75 m Anode (Rh), positive

Cooling water for anode

General Physical Principles S8 TIGER Operators Manual

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Continuous Spectrum When accelerated electrons collide with atoms of the metal target, they can be stopped on impact, in which case all their energy is converted into radiant energy, or they can be decelerated in steps, in which case a part of their total energy is released in the form of X-rays of greater wavelengths at each step until it is expended. The incident electron enters the electric field between the electrons and the nucleus of an atom and is deflected and decelerated by it at the same time. This process is repeated when the deflected electron enters the electric fields of other atoms.

Fig. 2-2: Production of continuous (white) radiation.

The waves of X-rays generated in this way are called continuous radiation because they form a con-tinuous spectrum of wavelengths.

S8 TIGER Operators Manual General Physical Principles

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Characteristic Spectrum High-energy electrons can also interact with the atoms of the metal target to produce another type of radiation called characteristic radiation because the wavelengths of the photons emitted are charac-teristic of the anode metal.

In this case, the incident electron collides with an electron of the first, innermost electron shell of an atom and knocks it out of its orbit. To restore stability to the energy state of the atom, the ejected elec-tron is replaced by an electron from an outer shell. Because the energy levels of shells increases with their distance from the nucleus of the atom, the transition of a replacement electron from an outer to an inner shell is accompanied by a loss in energy, which is released in the form of X-rays.

Fig. 2-3: Production of characteristic radiation simplified representation.


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Fig. 2-3 is a simplified representation of the process by which characteristic radiation is produced through the transition of electrons at the atomic level. In this diagram the conventional notation for the electron shells and the photons produced by the transition of their respective electrons has been adopted. K radiation is produced by an electron transfer from shell L to shell K, K by a transfer from shell M to shell K, and L by a transfer from M to L. Note that the photons have different characteristic wavelengths.

In fact, on closer examination of the atom and its electron shells, it can be seen that the shells are divided into subshells as shown in Fig. 2-4 below. For this reason, K radiation can be divided into K1 and K2 radiation, K radiation into K1 and K2 radiation and so on. The difference between the wave-lengths of photons produced by the transfer of electrons of different subshells within the same shell is very small.

Fig. 2-4: Subshells and their transferred electrons.


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In Fig. 2-5 below, the wavelength distribution of both continuous and characteristic radiation is shown as a function of intensity or the number of pulse counts per second. The characteristic peaks K1, Ka2 and K1 are clearly visible above the continuous spectrum. The point on the wavelength scale at which the continuous spectrum begins is known as the short wavelength limit (SWL) and corresponds to the radiation produced by the electrons that give up all their energy on the initial impact. Thus for a particular supply voltage, these electrons give rise to pho-tons of maximum energy (minimum wavelength). With an increase in supply voltage, the SWL as well as the point of maximum intensity of the continuous spectrum moves down the wavelength scale. In other words, an increase in operating potential produces a shift of the continuous spectrum in the di-rection of lower wavelengths and higher energy. On the other hand, the characteristic spectrum, be-cause it is characteristic of the anode metal, merely undergoes an increase in intensity (pulse count rate).

Fig. 2-5: Spectrum of an X-ray tube.


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The Bragg Equation The secondary X-ray waves emanating from a family of atom-containing planes in the crystal lattice structure are in phase and constructively interfere with one another when the Bragg condition is met. This is expressed in the equation

N= 2d sin where N is an integer multiple called the order of reflection, is the wavelength of the X-ray beam, d is the distance between the planes, and is the angle of deflection. The Bragg equation is derived in the following way.

Fig. 2-6: Fulfillment of the Bragg equation.


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Fig. 2-6 shows a monochromatic beam of X-rays incident on the surface of a crystal at an angle . P, Q and R represent a family of planes separated by the distance d. Plane P reflects AX in XD. Similarly, plane Q reflects BY in YE at the same angle . Although the beam penetrates many more planes we need only consider the top two.

Since Q is lower than P, the beam path BYE is longer than AXD by the amount GY + YH. This is called the path difference.

Since angle AXG = + angle PXG = 90 Then angle PXG = 90 - Since angle PXY = PXG + GXY = 90

Then angle GXY = Similarly, you can show that angle YXH =

From the triangle GXY, d

GYsin Therefore GY = d sin

From the triangle YXH, d

YHsin Therefore YH = d sin

Therefore the path difference (GY + YH) = 2d sin Now the two reflected rays will constructively interfere with one another, that is, they will be in synch, when the path difference is equal to the wavelength () or a multiple of it. Thus N= 2d sin . The Bragg equation is used in diffractometry to determine the nature of the irradiated specimen. Once the Bragg angle is determined, this can be used, together with the known wavelength, to calculate the distance d and thus the geometry of the unit cells of the lattice.


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Scintillation counter A scintillation counter measures ionizing radiation. The scintillator consists of a transparent crystal that fluoresces when struck by ionizing radiation. A sensitive photomultiplier tube (PMT) measures the light from the crystal. When a charged particle strikes the scintillator a flash of light is produced. The PMT is attached to an electronic amplifier and other electronic equipment to count and possibly quantify the amplitude of the signals produced by the photomultiplier. The association of a scintillator and pho-tomultiplier with the counter circuits forms the basis of the scintillation counter. The intensity of the light flash depends on the energy of the charged particles. Cesium iodide (CsI) in crystalline form is used as the scintillator for the detection of protons and alpha particles; sodium iodide (NaI) containing a small amount of thallium is used as a scintillator for the detection of gamma waves.

Proportional counter A proportional counter is a type of gaseous ionization detector. It works on the same principle as the Geiger-Mller counter, but uses a lower operating voltage. An inert gas is used to fill the tube, with a quench gas added as a stabilizer. A common proportional gas mixture is 90% argon, 10% methane, known as P-10. An incoming ionizing particle, if it has sufficient energy, liberates electrons from the atomic orbitals of the gas atoms, leaving an electron and positively charged atom (ion pair). As the charged particle travels through the chamber it leaves a trail of ion pairs along its trajectory. The elec-trons created in this process drift under the influence of the electric field toward the electrode (anode). At the same time, the positive ions drift towards the cathode, at much lower speed. A proportional counter differs from an ionization chamber in that the operating voltage is sufficiently high that the drifting electrons gain enough energy over a mean free path to create further ion pairs when they col-lide with other neutral atoms of the gas. The electrons created in these new events also drift toward the electrode and can create further ion pairs themselves. If the operating voltage is chosen carefully, each avalanche process occurs independently of other avalanches which derive from the same initial ionizing event. Therefore, even though the total number of electrons liberated can increase exponen-tially with distance, the total amount of charge created remains proportional to the amount of charge liberated in the original event.

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3 Introduction to the Instrument Overview of this Manual

Note

This manual covers the basic operation of the S8 TIGER spectrometer. You should be familiar with its contents prior to switching on the instrument.

This manual consists of several chapters. First the safety warnings are given, which are also listed in the Introductory User Manual (order number DOC-M80-ZXX031) and the General Safety Instructions (order number DOC-M90-ZXX006) The Introductory User Manual, including the safety warnings, and the General Safety Instructions are available in several languages. Please consult with your local Bruker AXS service organization for availability in your language.

This chapter describes the instrument, its components and basic operation modes.

The following chapter describes how to switch the spectrometer on and off. Further, there is an over-view of the basic operation of the touchscreen. And a QUANT-EXPRESS measurement is described. The servicing, maintaining and troubleshooting of the system is described in the subsequent chapters. The appendix of this book gives references that turn out to be quite handy during day-to-day operation of the instrument.

SPECTRAplus is the analytical software package that is delivered with the instrument. The S8 TIGER runs SPECTRAplus Version 2.0 and higher. The software is described in a separate manual (order number DOC-M80-EXX038). For unknown samples it is recommended to use QUANT-EXPRESS. QUANT-EXPRESS is the standardless method applying a fundamental parameter approach for the analytics. Basic QUANT-EXPRESS operation is described in a separate chapter.

Introduction to the Instrument S8 TIGER Operators Manual

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Overview of the Product The S8 TIGER is a wavelength dispersive spectrometer available in three power ratings:

The base instrument allows maximum settings of 50 kV and 50 mA, while the power is limited to 1 kW. The 1 kW version can be operated without external water cooling.

The intermediate system runs at 3 kW with 60 kV and 150 mA as voltage and current limits. The increase of the voltage to 60 kV allows a better detection of heavier elements.

The high power system allows operation at up to 4 kW. The maximum high voltage remains at 60 kV, but the current can be increased up to 170 kV, which is unique in the market. For light ele-ment detection this allows shorter measurement times.

The default configuration for all three power settings is identical: The spectrometer is equipped with a helium system for liquid samples, a 34 mm manual mask, a flow counter, a scintillation counter, and a 60 position cup loader with 10 cups mounted with 34mm masks. In addition it is equipped with the following analyzer crystals: XS-55, PET, and LiF200. The 0.23 and 0.46 collimators are also pre-installed. The purpose of the optical components is explained later in this chapter of the Operator's Manual.

You will also find 5 reference samples delivered with the instrument. The application and usage are, for example, trained during on-site and factory site training courses. For routine operation the SPEC-TRAplus software suite, S8 Tools, and remote access software is installed on the computer. QUANT-EXPRESS, a standardless evaluation module, is installed as trial version, which expires after 90 days. It is a powerful analysis package of unknown samples. If the QUANT-EXPRESS package was pur-chased, a permanent licence is installed.

Please note that your instrument may be ordered in a different configuration adapted to your particular analytical needs. It can be beneficial to install additional monochromators to boost system perform-ance. For example for petro-chemical applications we recommend the use of the XS-Ge-C; for geo-logical application the LiF220, and for cement application the use of both XS-CEM and XS-Ge-C. For the detection of boron, carbon, and nitrogen, XS-B, XS-C, and XS-N should be used, respectively.

Commercially, the following packages are available as factory installed options:

EasyLoadTM: An 75 position loader with two trays for 51mm rings, automatic liquid sample detec-tion, and 20 sample rings.

S8 TIGER Operators Manual Introduction to the Instrument

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SampleCareTM: An automatic mask changer with one closed position for goniometer protection during pump-down, a 28 mm and a 34 mm mask installed, and a Be foil tube window protection.

TouchControlTM: This is a hardware component, a touchscreen with a dedicated single board computer and a user interface for intuitive operation. It can be ordered with a great number of lan-guages that can be switched on-the-fly. The touchscreen software, S8 TOUCH, was specifically written with routine operation in mind. It is seamlessly integrated into to the SPECTRAplus software suite.

Please check your shipping and order information if which options were included in your instrument.

Overview of the Operation Principle Inside the spectrometer samples are irradiated by X-rays with energy of up to 60 keV1. Typically, the samples are measured in vacuum for best detection limits, especially for light elements. In case of liquid samples, or in case of loose powder samples, it is also possible to measure while applying a nitrogen or helium atmosphere. The X-ray beam originates from the X-ray tube impinges on the sam-ple which then sends out X-ray fluorescence. The X-ray fluorescence radiation is characteristic for each element of the periodic table. For its creation the energy of the primary beam needs to be larger than the characteristic excitation radiation. The S8 TIGER can probe to energies up to 60 keV1.

1 Please note: The S8 TIGER 1kW version can probe to energies up 50 keV.


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Fig. 3-1: S8 TIGER with EasyLoad and TouchControl.


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The X-ray fingerprints of the elements are detected by the S8 TIGER detectors. The measured in-tensities are used to determine the elemental concentrations.

The beam path is shown in Fig. 3-2. The spectrum of the primary beam can be changed by inserting a primary beam filter. This can be useful if the excitation spectrum should be biased, for example to excited heavier elements more easily. To reduce the erroneous signals and background, the sample beam is collimated and made parallel by a collimator mask and a collimator. The collimator mask can be changed automatically like all other components in the beam path. The collimator is labelled by its opening angle. This limits the beam divergence of the excited beam. Smaller values lead to a better energy resolution albeit a smaller intensity. There are up to four collimators available.

Fig. 3-2: X-ray beam path of the S8 TIGER.

Sample Filter wheel (primary beam filter)

X-ray source

Proportional counter (light elements)

Scintillation counter(heavy elements)

Vacuum seal

Collimator changer

Crystal changer

Mask changer


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After leaving the collimator the beam impinges on an analyzer crystal. Those crystals are organic or artificially produced multi-layers. Depending on the lattice spacing and obeying Braggs Law the X-ray beam is diffracted at certain angles. A total of eight crystal positions can be used. As a default, three positions are used for PET, XS-55, and LiF 200 analyzer crystals. A quick overview of the elemental range of those standard crystals is shown in Fig. 3-3. In addition, Bruker AXS offers a large variety of optional crystals optimized for specific applications. The number of options is continuously growing. Please contact your local application or sales representative for detailed and up-to-date information.

Fig. 3-3: Overview of the typical elemental range for the three standard analyzer crystals. For a more detailed periodic table, please, consult the appendix.


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The radiation from the analyzer crystal is detected by one of the two detectors. One detector is opti-mized for soft, one for hard radiation1. To reduce the background even further both detectors are equipped with soller slits (not shown in Fig. 3-2).

The detectors are mounted onto the 2-theta goniometer, the sample on the theta-goniometer. For the measurement the respective detector is either positioned at a given angular position (peak measure-ment) or it is moving during the measurement (scan measurement). The angular position of construc-tive interference is determined by Braggs Law. This means the 2-theta position of a peak depends both on the d-spacing of the analyzer crystal and the characteristic wavelength of the element probed. Since all elements are measured subsequently, the instrument is referred to as sequential X-ray spec-trometer.

The beam path is inside a housing to shield the user from X-ray radiation. A safety circuitry assures that the radiation can only be produced if both the spectrometer chamber is closed and the protective covers are installed. The S8 TIGER can be operated with a variety to sample magazines.

Warning

It is illegal to hamper or defeat the radiation protection system.

1 Light elements emit soft (= low energy) radiation.


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Instrument Components The S8 TIGER is a fully automated X-ray spectrometer, both operation and analysis can run with very little user interaction. In this manual we will focus on the general instrument operation.

All the connection lines and cables can be found at the back of the instrument. Through those lines you supply electricity and water. You can also connect a local area network via an Ethernet connec-tion. Depending on your configuration and application, there might be two gas hoses, one for supply-ing P-10 to the flow counter and one for supplying Helium or Nitrogen to the sample chamber.

From the front and either side of the instrument, see Fig. 3-4, you can see a field of LEDs that are illuminated when X-rays are produced. These are the X-ray warning lights. When standing in front of the spectrometer to the left you see the on and the off button, an emergency off switch and the gen-erator turn-on key switch. To the right are the touchscreen and the panel with four LEDs that display an abbreviated instrument status.

When you open the instruments top you can have a close look at the sample magazine and the sam-ple robot.

Warning Do not use the handle of the top cover to pull the instrument!

Towards the back left the sample chamber can be found. There are many magazine types available. The whole magazine and robotics is often referred to as the loader. Prior to the measurement the test specimen is placed into a sample container, like a ring or a cup, and subsequently this ring or cup is placed into the loader.


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Fig. 3-4: Front view of the S8 TIGER.

Touchscreen

Status LEDs On and Off

switches

X-ray warning light

X-ray warning light

Top cover


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Fig. 3-5: Inside the loader (sample magazine).

During operation, all side panels must be mounted, since they are part of the X-ray safety system.

During installation and system commissioning and in case of a service visit, panels will be removed. The internal arrangement of the instrument will be revealed.

Sample position

Sample grabber

Sample chamber


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Fig. 3-6: View on the instrument after removing the front and the right side panel with several components labelled.

Electronics control rack

Generator

Safety board

Spectrometer chamber

Status LEDs


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Fig. 3-7: View on the instrument after removing the front and the left side panel with several com-ponents labelled.

Safety board

X-ray warning light

X-ray tube


Back side of the generator

On/off switch panel


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Fig. 3-8: View on the 3 or 4kW version after removing the back and the left (viewed from front) side panel with several components labelled.

Vacuum pump

Bottom of X-ray tube


Mask changer drive Port for con-veyor belt

(open for ONLINE option)


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Fig. 3-9: View on the 3 or 4 kW version after removing the back and the right (viewed from front) side panel with several components labelled.

Electronics control rack

Water pump Vacuum pump

Refill port for de-ionized water

Electric power distribution and mains connection

Heat exchanger

Generator


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Illuminated Status Display

X-ray warning display Ready On Alarm Busy

Fig. 3-10: Status display

LED Guide Tab. 3-1: LED guide

Ready (orange)

permanently on blinking

generator heating current on, HV off, system is in measurement standby mode

On (green)


HV generator and control electronics turned on (see all LEDs)

Alarm (red)


system alarm system warning is pending

Busy (yellow)


measurement is running a ready flag is missing, data taking is interrupted

All LEDs blinking at a frequency of about 2 Hz thermal shut down active


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Measurement Execution Basics of the S8 TIGER This chapter describes how the instrument executes a measurement. Also, the motivation for some of the implementations is given.

Measurements in most cases are executed under vacuum, since the S8 TIGER is used to detect a wide range of elements. Depending on the atomic structure, photons of different energies are emitted. The lighter the element, the smaller the energy of the most energetic photon emitted. The (soft) X-ray radiation of light elements is readily absorbed in air.

To speed up measurement time, the space is separated into two chambers: the sample chamber and the spectrometer chamber, which houses most of the optical components and the detectors. During loading and unloading the two chambers are separated, so only the relatively small sample chamber needs to be evacuated or flooded with air. However, after the initial turn-on also the spectrometer chamber needs to be evacuated.

In case fluids are measured, one typically floods the sample chamber with Helium (recommended), in some cases with Nitrogen. In most cases, if a liquid is put under vacuum, it starts to evaporate. This would soil the sample chamber. In addition, often not enough sample material might be left for analy-sis. In both Helium modes the spectrometer chamber remains evacuated. The two chambers are separated by a patented highly X-ray transparent vacuum seal. Helium is very transparent to X-rays. Depending on your sample you can chose between two Helium modes. If you decide to measure loose powders it is also strongly recommended to operate in Helium mode.


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Tab. 3-2: Overview of the S8 TIGER atmospheric measurement modus. Please note that some modes are optional.

Mode Samples Remarks Vacuum Metals,

fused beads, pressed pellets glass

Compact solid samples to achieve best sensitivity for light elements

Separated vacuum Pressed powders (dusty samples)

The vacuum seal protects the goniometer and com-partments against dust particles released from the sample. IMPORTANT: It is strongly recommended to prepare pressed pellets as stable as possible by using the appropriate binder and applying best pressure

Helium (reduced pressure)

Liquid samples Oils, water Loose powders in a cup with polymer film

To avoid sample evaporation and the resulting con-tamination and/or damages, liquid samples must not be measured under vacuum. The helium mode with reduced pressure is recommended for liquids with a high boiling point. The helium pressure is reduced to gain better intensity for light elements and to keep helium consumption low.

Atmospheric Helium Liquid samples automotive fuels or solvents

All liquid samples with a low boiling point, like fuels, must be run under atmospheric helium to avoid boil-ing and evaporation of the sample.


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Several pressure sensors monitor the vacuum continuously. Only after the pressure is sufficiently low, is possible to start a measurement.

The S8 TIGER is a wavelength-dispersive spectrometer. Intensities for individual wavelengths are determined in what is also known as Bragg-Brentano geometry with, in our case, the sample acting as radiation source. The analyzer crystal and detector are moved in a fixed angular relationship of 1:2. This gives great flexibility to the instrument. It can be adjusted to almost any new analytical task. On the other hand, this also means that measurements of different samples are executed in sequence. So, before the sample is in measurement position, the instrument has to know for which elements to probe. Based on this input, the optical components (beam filter, mask, collimator, analyzer crystal, and detector) are moved into position while the chamber is being evacuated. Most motions can be exe-cuted in parallel.

Once in position, the measurement starts immediately. All components move in parallel to get ready for the measurement. After all measurement tasks are finished, the sample is removed from the sam-ple chamber. During sample transfer, no X-rays are produced for your safety. There are two types of measurements: Peak Measurement (faster; only the intensity at one position is measured) and Scan Measurement (the goniometer performs a coupled scan, the peak shape and intensity over an angular range is determined).

More background on XRF analysis and some instrumentation background can be found in the Bruker AXS publication Introduction to X-ray Fluorescence Analysis (DOC-M84-EXX001). Additional refer-ences are given therein.

Note

Please consult the Introductory User Manual for an in-depth description of the safety sys-tem.


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Flow Chart Showing Standard Operation

If no sample in measurement positionGrabber moves to sample position (xy)And moved down (z) to sample height.

Checks if sample is detected.

Turn on magnetization.

Move up (z).

Error message

Move to sample input position (xy).

Sample chamber ready signal

Error

Wait.

YES NO

Open shutter.

De-magnetize (leave sample).

Move down.Check if height is okay.

Move in vacuum seal. Note: Separates spectrometer chamber from sample chamber.

Ramp down I, V of HV generator for X-ray.

Flood sample chamber with air. Note: Big spectrometer chamber remains evacuated.

Move grabber to max. position.Move grabber to park position (xy).

YES NO

YES NO

Continued on the next page.


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Continuation of flow chart: Move grabber to max. position.

Move grabber to park position (xy).

Close vacuum seal.

Evacuate sample chamber.

Wait ~ 2s.

Move goniometer and optics in position.

X-ray OnRamp up HV for X-ray tube.

Check if V, I for X-raytube ready and stable.

Check if gas flow is okay(if flow counter is installed).

Pump and checkif vacuum okay.

IF NOT IF NOT IF NOT

Error and stopmeasurement.



Check target positions are reached.

IF OK

Execute measurement program (method).

End measurement.

Move grabber to sample input position (xy).

Move in vacuum seal.

Ramp down X-ray HV and current.

Flood sample chamber with air.

Remove sample. Fig. 3-11: Flow chart showing standard operation.


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Network Configuration The SPECTRAplus PC and the S8 TIGER are connected together via a network. Depending on your network configuration this may be a simple cable from the PC to the S8, or the devices may be con-nected via a hub or switch. Alternatively both devices may be connected to your local-area-network (LAN). The S8 TIGER will request an IP address via DHCP, and if a DHCP server is not available, it will assign itself an automatic private IP. It is recommended that the SPECTRAplus PC is configured for DHCP to ease any network configuration problem. The network settings of the devices leaving the factory are guaranteed to work. If you need to reconfigure the devices for your network please contact your Bruker representative for advice and instructions.

Fig. 3-12: S8 TIGER SPECTRAplus PC network connection.

C:\Program Files\SPECPlus SPECTRAplus programs e.g. Loader.exe Eval2.exe etc.

C:\ Embedded OS TouchControl Measurement Server

D:\SPECplus Data files, log files, cali-bration files, databases, measurement methods, format methods etc.

Connect via SPBrowser e.g. T:\SPECplus


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The SPECTRAplus PC accesses data on the S8 TIGER via a Windows mapped drive. It is recom-mended to use the SPBrowser program map the S8 drive automatically.

Fig. 3-12 shows an overview of the software and data files for the PC-S8 system. It is important to note that there is a separation between data files and programs. This is to allow the S8 TIGER to work as a stand alone instrument, allowing routine measurements even when the PC is switched off.

Use of an External PC You can operate the S8 TIGER with TouchControl on the touchscreen or with the measurement software SPECTRAplus on an external PC via network.

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4 Switching the Instrument On and Off

Switching On Auto Start Up of the S8 TIGER 1. Verify the instrument is connected to a 40A 208-240V AC supply.

2. Check that the external cooling water system is operating correctly. All valves connecting to the instrument are open and hoses correctly connected to the S8 TIGER.

3. Check the P-10 and helium supply (if used) is turned on and set correctly. The P10 should be set to 0.5 bar (~7 PSI). Helium should be set to 2 bar (~29 PSI).

4. The system configuration should be set in the Default parameters pane to Airlock mode = Spec-trometer mode (Standby parameters) and vacuum with seal (Mode). The default settings see in Fig. 4-1.

5. Press the green power-on button on the front of the spectrometer (Fig. 4-2). All four lights will come on for about 30 sec. If the lights do not come on verify the STOP button is out by turning it clockwise then press the green button again.

Note

For this procedure to work auto setup1 must be enabled. This is the default setting.

S8 TIGER Operators Manual DOC-M80-EXX032 V3 Complete

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Transcript of S8 TIGER Operators Manual DOC-M80-EXX032 V3 Complete