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10-015490-01EN, Rev. 2, June 2020

Set Up and Operation

3. Set Up and Operation

This chapter provides information for turning on and off the BTX III XRD analyzer
and preparing and testing samples.

3.1

Connecting AC Power to the BTX III

The BTX III analyzer receives AC power through the External Power connector.

To connect AC power

If an unauthorized power supply cord is used to power the instrument, Olympus
cannot guarantee the electrical safety of the equipment.

Hold the power supply output plug in the orientation shown, and then insert it
into the rear panel Power connector (see Figure 3-1 on page 36).

CAUTION

Содержание BIX III

Страница 1: ...r User s Manual This instruction manual contains essential information on how to use this Olympus product safely and effectively Before using this product thoroughly review this instruction manual Use...

Страница 2: ...ein and corresponds to the version of the product manufactured prior to the date appearing on the title page There could however be some differences between the manual and the product if the product w...

Страница 3: ...Safety Signal Words 7 Note Signal Words 8 Safety 9 Warnings 9 Richtlinien f r den Strahlenschutz im deutschsprachigen Raum 11 Deutschland 11 sterreich 11 Schweiz 12 Equipment Disposal 12 CE European C...

Страница 4: ...1 Connecting AC Power to the BTX III 35 3 2 Turning On or Off the BTX III 37 3 3 Preparing a Sample for Analysis 38 3 4 Loading a Sample 39 3 5 Testing a Sample 45 3 6 Unloading a Sample 48 4 Local Ar...

Страница 5: ...61 5 3 3 Manager Access Workflow 64 5 3 3 1 Mineral Config Tab 65 5 3 3 2 Mode Setup Tab 68 5 3 4 Changing the User Interface Language 73 Appendix A Specifications 75 Appendix B About Powder XRD Test...

Страница 6: ...Table of Contents vi 10 015490 01EN Rev 2 June 2020...

Страница 7: ...evice DHCP dynamic host configuration protocol EFUP environment friendly use period FWHM full width at half maximum HVPS high voltage power supply LAN local area network OSS open source software PXRD...

Страница 8: ...10 015490 01EN Rev 2 June 2020 List of Abbreviations viii...

Страница 9: ...ols are attached to the BTX III X ray diffraction analyzer see Figure i 1 on page 1 If any of the labels or symbols are missing or illegible please contact Olympus Figure i 1 X ray warning labels The...

Страница 10: ...CE marking is a declaration that this product conforms to all the applicable directives of the European Community See the Declaration of Conformity for details Contact your Olympus representative for...

Страница 11: ...ly Use Period EFUP The EFUP is defined as the number of years for which listed controlled substances will not leak or chemically deteriorate while in the product The EFUP for the BTX III has been dete...

Страница 12: ...10 015490 01EN Rev 2 June 2020 Labels and Symbols 4...

Страница 13: ...Do not use the BTX III analyzer for any purpose other than its intended use It must never be used to inspect or examine human or animal body parts Instruction Manual This instruction manual contains e...

Страница 14: ...its required DC input power from the BTX III analyzer s AC adaptor Always use equipment and accessories that meet Olympus specifications Using incompatible equipment could cause equipment malfunction...

Страница 15: ...D analyzer All safety messages that follow this symbol shall be obeyed to avoid possible harm Shock hazard caution symbol This symbol is used to alert the user to potential electric shock hazards All...

Страница 16: ...ction of part or all of the product or loss of data Do not proceed beyond a CAUTION signal word until the indicated conditions are fully understood and met Note Signal Words The following note signal...

Страница 17: ...e safety warnings on the instrument and in this instruction manual If the equipment is used in a manner not specified by the manufacturer the protection provided by the equipment could be impaired Do...

Страница 18: ...e rating label If an unauthorized power supply cord is used to power the instrument Olympus cannot guarantee the electrical safety of the equipment High Voltage The BTX III XRD analyzer uses a 30 kV h...

Страница 19: ...chtig 3 R V Sorgen Sie daf r dass in Ihrem Betrieb mindestens ein Strahlenschutzbeauftragter mit Fachkunde R2 nach der deutschen R ntgenverordnung verf gbar ist Dar ber hi naus sollten Sie die Bediene...

Страница 20: ...wie Handlungs und Arbeitsanwei sungen sind dem Bedienpersonal jederzeit zur Verf gung zu stellen Es wird empfohlen jeden Bediener mit einem amtlichen Dosimeter auszur sten Schweiz Der Betrieb von R nt...

Страница 21: ...E marking indicates compliance with the above directives In accordance with European Directive 2012 19 EU on Waste Electrical and Electronic Equipment WEEE this symbol indicates that the product must...

Страница 22: ...munications Commission KCC KCC South Korea Community This device complies with the requirements of KN 61000 6 2 and KN 61000 6 4 concerning electromagnetic compatibility The KCC marking indicates comp...

Страница 23: ...tection against harmful interference when the product is operated in a commercial environment This product generates uses and can radiate radio frequency energy and if not installed and used in accord...

Страница 24: ...e de la classe A est conforme la norme NMB 001 du Canada Packing and Return Shipping If the BTX III is not returned in its transport case it could be damaged during shipping Olympus reserves the right...

Страница 25: ...ALITY AND PERFORMANCE OF THE OSS IS WITH YOU SHOULD THE OSS PROVE DEFECTIVE YOU ASSUME THE COST OF ALL NECESSARY SERVICING REPAIR OR CORRECTION Some of the OSS licenses associated with this product ma...

Страница 26: ...ntended solely as a teaching aid and shall not be used in any particular application without independent testing and or verification by the operator or the supervisor Such independent verification of...

Страница 27: ...wer X ray source and 2 D charge coupled device CCD detector to obtain XRD data The BTX III analyzer incorporates the following independent safety protection circuits Power key switch Key must be inser...

Страница 28: ...10 015490 01EN Rev 2 June 2020 Introduction 20...

Страница 29: ...Analyzer Overview This chapter provides an overview of the BTX III X ray diffraction analyzer and its accessories 1 1 Packing List Table 2 on page 21 lists the BTX III components Table 2 BTX III compo...

Страница 30: ...xternal sample shaker assembly Accessory kit 1 Micro spatula 2 Ball driver 3 Power keys 2 4 USB flash drive loaded with software database and documentation 5 Sample cells 1 Kapton and 1 Mylar 6 Sample...

Страница 31: ...and top panels are where all BTX III controls indicators and the sample chamber are located see Figure 1 1 on page 23 and Table 3 on page 24 Figure 1 1 BTX III front panel 7 Sample crusher 8 Sample si...

Страница 32: ...e 24 Figure 1 2 Power key switch On 1 2 2 Keypad The keypad enables you to make selections on the display to set up and run tests and save results see Figure 1 3 on page 25 Table 3 BTX III front top p...

Страница 33: ...system power in an emergency or cancel a selection when using the keypad and main menu to set up tests see Figure 1 4 on page 25 Figure 1 4 Stop Emergency Shutoff button 1 2 4 LED Indicators The LED i...

Страница 34: ...e carrier see Figure 1 6 on page 26 Figure 1 6 Sample chamber assembly 1 2 6 Display The display shows selections for setting up and monitoring tests see Figure 1 7 on page 26 Figure 1 7 Display 1 3 R...

Страница 35: ...l Shaker Port for connecting the external sample shaker The shaker is used to load and unload samples from the BTX III sample carrier 3 Ethernet Port for connecting the BTX III to an Ethernet network...

Страница 36: ...10 015490 01EN Rev 2 June 2020 Chapter 1 28...

Страница 37: ...adiation dose ALARA Time The most direct way to reduce radiation dose is to reduce the time spent working with or in the vicinity of radiation sources If the exposure time is cut in half the dose will...

Страница 38: ...the system housing and constructed in such a way that no measurable radiation is detected during operation No beam alignment nor X ray beam calibration by the operator is required There is no reason f...

Страница 39: ...features Label Safety feature 1 Sample chamber interlock The X ray beam only operates when the sample carrier is properly inserted into the system If the carrier is removed while the system is in ope...

Страница 40: ...ned A safety interlock switch could be triggered by removing the sample carrier during a sample analysis 4 Power key switch The power key switch has ON and OFF positions The key must be inserted and i...

Страница 41: ...radiation levels less than 0 2 mR h This level is well within acceptable levels of exposure to the general public When properly set up and operated there is no exposure in excess of the typical dosag...

Страница 42: ...diation level measurements Measurement point Measured radiation level in C kg Distance from surface cm Comments A 0 0129 2 Front top panel B 0 0129 2 Left side of case C 0 0129 2 Front side of case D...

Страница 43: ...ng AC Power to the BTX III The BTX III analyzer receives AC power through the External Power connector To connect AC power If an unauthorized power supply cord is used to power the instrument Olympus...

Страница 44: ...10 015490 01EN Rev 2 June 2020 Chapter 3 36 Figure 3 1 Power plug and connector 2 Plug one end of the AC power cord firmly into the power supply see Figure 3 2 on page 36 Figure 3 2 Power supply...

Страница 45: ...e message Welcome to BTX Booting Please wait After about a minute the display reads Cooling to 45 Current temp temperature After the detector cools to 45 C the menu appears see Figure 3 3 on page 37 F...

Страница 46: ...small particles generally do not perform well within a standard BTX III sample cell The particles tend to stick to one another and not convect as they should If you encounter this condition contact O...

Страница 47: ...here are four components of a sample cell see Figure 3 6 on page 39 An inner cell window comprised of a polymer window on a metal frame with a notch at the top A spacer which is assembled between the...

Страница 48: ...3 7 on page 40 Figure 3 7 Sample carrier The BTX III analyzer is supplied with an external shaker assembly to ease sample loading and unloading see Figure 3 8 on page 40 The external shaker assembly i...

Страница 49: ...ple carrier see Figure 3 10 on page 41 Figure 3 10 Removing the sample carrier To assemble a cell 1 Lay the inner window down first see Figure 3 11 on page 42 Make sure that the polymer film faces up...

Страница 50: ...he cell assembly are aligned with the holes in the sample carrier see Figure 3 12 on page 42 5 Replace the holding screws being very careful not to puncture the polymer window material 6 Tighten the h...

Страница 51: ...el see Figure 3 13 on page 43 Figure 3 13 External shaker plug connected 2 Insert the sample carrier into the external shaker and gradually load a small amount of material enough to fill the gap creat...

Страница 52: ...he external shaker vibrates to aid in loading the sample 4 Adjust the shaking amplitude using the Left arrow and Right arrow buttons 5 To save the selected shaking amplitude value press the Check butt...

Страница 53: ...le 1 Insert the sample carrier into the sample chamber making sure that side A is oriented toward the right side of the system see Figure 3 15 on page 45 Figure 3 15 Inserting the sample carrier 2 Loc...

Страница 54: ...46 Table 8 Running modes Menu level one Menu level two Level two choice Comments Start acquisition Choose Mode Default Uses the default test mode that has been set up by the administrator in the Swif...

Страница 55: ...n Press the Stop button once Shaking X to quit Initiates vibration of the external shaker assembly assuming it is connected Press the Stop button on the keypad to terminate external shaking Adjust the...

Страница 56: ...mple carrier out of the sample chamber To unload a sample from the sample cell Remove the majority of the material with the aid of the external shaker assembly OR 1 Using a 1 5 mm hex driver carefully...

Страница 57: ...f the two following methods Connect an Ethernet cable to the Ethernet connector to establish a wired LAN Connect a wireless LAN dongle to the USB connector to establish a wireless LAN Your PC tablet o...

Страница 58: ...setting of the BTX III is WIRED ON Ethernet 1 Make sure the BTX III is on and the Main menu is displayed 2 Briefly press both the Left arrow and Right arrow buttons at the same time to display the Adv...

Страница 59: ...o your LAN through the Ethernet Connector When the LAN is set to WIRED ON the BTX III is configured to connect to your LAN through the Ethernet connector To connect to your LAN through the Ethernet co...

Страница 60: ...DHCP Menu to view the network assigned IP address see Figure 4 4 on page 52 The network assigned IP address must be used in your Web browser to access the BTX III software Figure 4 4 Network assigned...

Страница 61: ...he changes and restart the BTX III The BTX III restarts with the new DHCP configuration and begins broadcasting a WLAN 4 4 Connecting your PC to the WLAN Through the wireless LAN dongle the BTX III br...

Страница 62: ...find the serial number associated with your BTX III see Figure 4 7 on page 54 Figure 4 7 BTX III network broadcasting 2 Connect your PC to the BTX III see Figure 4 8 on page 55 You are now ready to se...

Страница 63: ...10 015490 01EN Rev 2 June 2020 Local Area Network Communication 55 Figure 4 8 BTX III network selected left and connected right...

Страница 64: ...10 015490 01EN Rev 2 June 2020 Chapter 4 56...

Страница 65: ...iftMin functionality 5 1 Opening and Closing the SwiftMin Software User Interface The SwiftMin software UI runs in a web browser of your choice To open the SwiftMin software user interface 1 Start a w...

Страница 66: ...re provides two user access levels Default Manager The Default access level is used for real time operation of the BTX III analyzer The Manager access level also provides real time operational capabil...

Страница 67: ...yed when the software starts up The Results and About screens are selectable 5 2 2 Manager Access Manager access is password protected Five screens are available Live Operator Mode Setup Mineral Confi...

Страница 68: ...password in the Enter Password dialog box and click Ok see Figure 5 3 on page 60 Figure 5 3 Enter Password dialog box To log out of Manager access 1 Click the icon in the upper right corner of the scr...

Страница 69: ...test parameters such as the SwiftMin and SwiftMin RIR databases number of exposures piezo volume and network parameters Mineral Config not available with default access Used to quickly edit SwiftMin R...

Страница 70: ...iquely identify the test in the Results screen For example if you enter BakerShaleA420 in Sample Name 20 in Info Field1 and 3X in Info Field2 the test name will appear in the results data as BakerShal...

Страница 71: ...re User Interface 63 Figure 5 6 Date Mode dialog box 3 Select a mode If you do not select a mode the last selected mode is used 4 Click Apply 5 In the list that appears choose the date and result that...

Страница 72: ...lighted sample to the BTX III analyzer 5 3 3 Manager Access Workflow Manager access includes all of the Default access level functionality and you can also configure mineral databases and test paramet...

Страница 73: ...1 Click the Mineral Config tab 2 Click the down arrow in the SwiftMin DB selection box and choose a database see Figure 5 8 on page 66 After you select a database the mineral list for that database is...

Страница 74: ...base left and editing the mineral list right To upload a csv or txt mineral database 1 Click Upload Database to open a file explorer window see Figure 5 9 on page 67 2 In the file explorer navigate to...

Страница 75: ...tMin Software User Interface 67 Figure 5 9 Upload database To download a csv or txt mineral database 1 Click Download Database 2 In the dialog box click the down arrow beside the database you want to...

Страница 76: ...erials are correct 5 3 3 2 Mode Setup Tab The Mode setup tab is where you set up the test modes for selection in the Live Operator screen You can change default test mode parameters or add edit or del...

Страница 77: ...e the default database 1 Click on a default database and select a different database see Figure 5 11 on page 69 2 Click Save Figure 5 11 Changing the default database To change any of the other defaul...

Страница 78: ...lay the Add New Mode dialog box Figure 5 12 Add New Mode button 2 In the dialog box select the Add New Mode field and type the name of the new mode see Figure 5 13 on page 71 3 Select the default data...

Страница 79: ...10 015490 01EN Rev 2 June 2020 SwiftMin Software User Interface 71 Figure 5 13 Add New Mode dialog box To edit an existing mode 1 Click an Edit button see Figure 5 14 on page 72...

Страница 80: ...15 on page 72 select the default database see To change the default database on page 69 3 Change any of the other default settings see To change any of the other default values on page 69 4 Optionally...

Страница 81: ...lete button see Figure 5 16 on page 73 Figure 5 16 Delete buttons 5 3 4 Changing the User Interface Language The Language tab enables you to change the language in the UI To change the user interface...

Страница 82: ...10 015490 01EN Rev 2 June 2020 Chapter 5 74...

Страница 83: ...cations Table 9 BTX III specifications Parameter Specification XRD resolution 0 25 2 FWHM XRD range 5 55 2 Detector type 1024 256 pixels 2 D Peltier cooled CCD Sample grain size 150 m crushed powder 1...

Страница 84: ...10 015490 01EN Rev 2 June 2020 Appendix A 76...

Страница 85: ...al lattice the abundance of the phase in the sample and the geometry of the system A general rule of thumb for powder XRD is that at least 106 grains are needed to provide appropriate particle statist...

Страница 86: ...mple A a still sample partial diffraction rings and Laue spots are observed In example B with granular convection complete diffraction rings are observed what is known as a perfect powder pattern Figu...

Страница 87: ...on analyzer on the USB flash drive This appendix includes instructions on installing the software and using it to verify alignment of the system using a quartz sample not supplied To install XPowder 1...

Страница 88: ...IFDATA database 1 Click Database Database Install 2 In the Drive list click the down arrow to locate the USB flash drive see Figure C 2 on page 81 3 Under Click database file select the Difdata txt fi...

Страница 89: ...5490 01EN Rev 2 June 2020 Data Analysis 81 Figure C 2 Database install To load test data 1 Click File Open 2 In the file type list change the file type to x y ascii txt asc xy x_y see Figure C 3 on pa...

Страница 90: ...ure C 3 Open File dialog box 3 Locate the file containing your quartz sample results Ensure the file name ends with film txt 4 Click Open to display the XPowder home screen and the superimposed Wavele...

Страница 91: ...tube type and automatically displays only on initial software setup 5 In the X ray tube anode list select either Co or Cu 6 The selection depends on the type of X ray tube in your system 7 Click OK T...

Страница 92: ...ogram appears 5 In the diffractogram click within the blue background subtraction area to decrease the amount of background subtraction see Figure C 6 on page 84 The purpose of decreasing or increasin...

Страница 93: ...area 7 In the Matching criteria box select 2 reflections option both the radio button and check box 8 Click Search The search results are displayed in the XPowder window with a dialog box superimpose...

Страница 94: ...er software identifies the first crystal phase that best matches the pattern 10 In the phase list click the check box of the highlighted phase to identify the next phase most likely to fit the pattern...

Страница 95: ...d phase 12 Click Display card to inspect the phase details see Figure C 10 on page 87 Figure C 10 Phase detail display card 13 In the XPowder window click Quantitative LS RIR Database Cards to view a...

Страница 96: ...10 015490 01EN Rev 2 June 2020 Appendix C 88 Figure C 11 Quantitative screen 14 To view a log report click File Save log file as TXT to generate a text file record of the session...

Страница 97: ...points 34 Figure 3 1 Power plug and connector 36 Figure 3 2 Power supply 36 Figure 3 3 Menu 37 Figure 3 4 Crushing a sample 38 Figure 3 5 Sample sieves 39 Figure 3 6 Sample cell window components 39 F...

Страница 98: ...5 9 Upload database 67 Figure 5 10 Download Database dialog box 68 Figure 5 11 Changing the default database 69 Figure 5 12 Add New Mode button 70 Figure 5 13 Add New Mode dialog box 71 Figure 5 14 E...

Страница 99: ...ng label 2 Table 2 BTX III components 21 Table 3 BTX III front top panel items 24 Table 4 BTX III rear panel connectors 27 Table 5 BTX III radiation safety features 31 Table 6 LED behavior 33 Table 7...

Страница 100: ...10 015490 01EN Rev 2 June 2020 List of Tables 92...

Страница 101: ...ipment 12 Dynamic Host Configuration Protocol 50 E EMC directive compliance 15 equipment disposal 12 Ethernet connector 27 51 European Community CE 13 external shaker 27 40 43 47 48 F FCC USA complian...

Страница 102: ...tes 8 IMPORTANT 8 NOTE 8 TIP 8 safety 7 CAUTION 8 DANGER 7 WARNING 8 software user interface 57 specifications 75 Stop Emergency Shutoff button 24 25 37 Strahlenschutzbeauftragter Deutschland 11 Strah...

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