Rigaku MiniFlex 600 Instruction Manual
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Rigaku MiniFlex 600 Instruction Manual

Benchtop x-ray diffractometer
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Benchtop X-ray Diffractometer
Instruction Manual
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Summary of Contents for Rigaku MiniFlex 600

  • Page 1 Benchtop X-ray Diffractometer Instruction Manual This image is an example of MiniFlex series. The actual product may differ from the image.
  • Page 2 This manual described in it may not be disclosed to a third party or copied, in whole or in part, without the written consent of Rigaku Corporation. In no event will Rigaku Corporation be responsible for the results of the use of this manual. As a rule, one set of the instruction manual has to be purchased for each product.

  • Page 3: Table Of Contents

    Contents Overview ......................1 Overview of MiniFlex 600 ................... 1 Optical System using SC ................... 2 Configuration ...................... 3 Standard Configuration ....................3 Names of Parts ......................4 List of Shipped Items ....................8 Specifications ....................... 9 X-Ray Generator ...................... 9 Tube shield ......................
  • Page 4 Replacing the X-ray Tube (Procedures required when cleaning filter or replacing tube) 91 Removing and installing the X-Ray tube ............91 Disassembling the X-ray tube and cleaning the filter ..........93 Cleaning and Further Information ................94 Confirming the Alarm Information ................95 MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 5 Optics alignment and notes on monochromator ............103 Arrangement of slits ..................... 104 Item No. 2005L101 / L102 / L201 / L202 / L301 / L302 / L401 / L402 Manual No. ME14992A03 2014. 02 (3rd Edition) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 7: Overview

    Overview Before starting to use the MiniFlex 600 Benchtop X-ray Diffractometer (hereon called MiniFlex 600), be sure to read this instruction manual thoroughly. Also, be sure to read the "Guidelines for safe use of the Benchtop X-ray Diffractometer" (ME11594*). Overview of MiniFlex 600 The MiniFlex 600 is a successor of the MiniFlex Benchtop X-ray Diffractometer (XRD) series.

  • Page 8: Optical System Using Sc

    Overview Optical System using SC Fig. 1.1 outlines the optical system of MiniFlex 600 using the scintillation counter. This optical system adopts focusing geometry used in powder XRD generally and irradiates the sample with divergent X-rays limited by a divergent slit. The features...

  • Page 9: Configuration

    These components may be required to be prepared by the user or distributor due to warranty issues. If an auto-transformer or an external heat exchanger is required, contact the sales representative who you purchased the instrument from. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 10: Names Of Parts

    Data output X-ray θ X-ray tube Electronic Cable circuit panel Goniometer (ECP) Angle control High voltage generator X-ray generator Computer (b) Block diagram Fig. 2.1 Appearance and block diagram of MiniFlex 600 (including optional components) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 11 Air vent Power source (inside) Power ON/OFF switch LAN cable outport Cooling water （〇: OFF , ｜: ON） IN/OUT Front view Right side view Rear view Fig. 2.2 Appearance of main unit and names of parts MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 12 Control driver Top view (perspective drawing) Beam stop (partition to prevent leakage) X-ray tube Tube shield X-ray shutter Goniometer Detector (SC) + monochromator Front view (perspective drawing) Fig. 2.3 Major components and names of parts MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 13 Names of Parts Fig. 2.4 Dimensions of main unit (weight: approx. 80 kg) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 14: List Of Shipped Items

    Inner diameter 9 mm x Outer diameter 15 mm Fixing jig for breaker OFF 1 set * For countries outside of Japan, these items may be required to be prepared by the user or distributor. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 15: Specifications

    10 mm, 5 mm (optional), 2 mm (optional) Auxiliary DS This is a variable slit to limit the width of X-ray beam irradiated on sample to be approx. 20 mm (sample width) at low angle area 1.25°, 0.625° (optional), 4.2° (optional) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 16: Detector (Sc)

    A flow rate of 3.0 l/min. or less on the water-drainage side is detected. Cooling water hose: φ9 inner diameter, φ15 outer diameter, 10 m in length each (Tetron braided.) Two cooling water hose bands are included. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 17: X-Ray Tube

    1024 x 768 resolution or higher CD-ROM drive: Required Keyboard: Required Mouse: Required LAN port: One port Printer Ink-jet color printer (compatible with A4 size) LAN cable Standard Software MiniFlex Guidance PDXL Basic Software Integrated Intensity Calculation MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 18: Optional Accessories

    Effective window size: 13 mm (W) × 20 mm(H) Dimensions: 80 mm (L) Included accessory: Beam stop Variable knife edge The following items are specifications that differ from SC: 2θ measurement range: +2° to +140° Slit: 8 mm (also called AS: Antiscatter slit) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 19: Installation Condition

    To install MiniFlex 600, the following conditions must be satisfied: Installation Room The MiniFlex 600 is a benchtop installation type equipment. Prepare a bench or a desk with the space and load limit specified below, and install it on a stable bench.

  • Page 20: Preparing Power Supply

    ・ No surge/noise generating equipment must be connected to the wiring for MiniFlex 600. ・ Connect the power source and MiniFlex 600 main unit directly with a cable. Do not insert a switch or any other power-consuming device in between.

  • Page 21: Cooling Water

    Install the equipment so the drainage port is located within 20 cm from the floor (drained by natural discharge). Others The cables of the equipment should be protected in a duct or cover to prevent them from being damaged. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 23: Installation Of Miniflex600

    Place the O-rings (two, included within the storage box) on the upper ② side of the tube shield. Without the O-rings, the cooling water may leak out. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 24: Connecting The Cooling Water Hose

    Attach the IN and OUT labels on the end of the cooling hoses. MiniFlex 600 (rear side of main body) Cooling water supply source Cooling water hoses Fig 5.3 Connecting the Cooling Water Hoses MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 25: Installing The Scintillation Counter (Sc)

    ・There are two types of parts for transportation. The type differs depending on the system configuration (see Fig. 5.4a and Fig. 5.4b). MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 26 Loosen the receiving slit box fixing screws, and slide the receiving slit ② box to the direction of the SC so it is positioned right next to SC. Slide it to the SC side Receiving slit box fixing screws Fig. 5.7 Moving the receiving slit box MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 27 HV value. Before mounting the upper cover of the enclosure, take note and remember this value. This HV value will be used as the initial HV value of the Fig 5.10 Label attached on SC MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 28: Installing The D/Tex Ultra (Optional)

    D/teX Ultra at this position. Fig. 5.11 Position to install D/teX Ultra Fig. 5.12 Installing the D/tex Ultra MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 29 Low and High discriminator value. Take note and remember these values before mounting the upper cover of the enclosure. For the figure below, the discriminator value is indicated as Low=37 and High=53. Record as BL=Low=37, WD=High(53)-Low(37)=16. Fig. 5.16 Label attached on D/teX Ultra MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 30: Installing The Beam Stop

    Installing and retracting the variable knife edge Installing the variable knife edge Remove the slider retracting screw from the variable knife edge. Variable knife edge Slider retracting screw Fig. 5.18 Removing the slider retracting screw MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 31 Marker on sample holder Fig. 5.20 Aligning the markers Tighten the fixing screw with hex wrench and fix the variable knife edge in place. Fixing screw Fig. 5.21 Fixing the variable knife edge in place MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 32: Retracting The Slider

    When removing the slider retracting screw, hold the variable knife edge by hand and let the slider slide down slowly. Be sure to remove the slider retracting screw when the optics alignment is completed. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 33: Installing The Ds And Ihs (Length Limiting)

    Connecting with Computer Connect the LAN connection port of the computer to the LAN connection port on the rear side of MiniFlex 600 main unit (inner side) with the LAN cable. If there are more than two LAN connection ports on the PC side, connect to the specified LAN connection port.

  • Page 34: Installing The Software

    Calculation” are used for the adjustment of the equipment, measurement, and analysis. This instruction manual includes only the minimum description of the software. For details, refer to the Help menu or instruction manual of each software. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 35: Setting And Adjustment

    Confirm it from the space between the incident cover and the X-ray tube. Either the label of 5.0 deg or 2.5 deg can be confirmed. Incident cover Check the label Fig. 6.1.1 Confirming the incident Soller slit MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 36: Types Of Receiving Soller Slit

    ・When “High resolution” is selected as incident Soller slit, the receiving soller slit is 2.5deg. Optional types of receiving Soller slit (other than those included with the system) can be replaced by the user as well. Receiving slit box Fig. 6.1.2 Receiving Soller slit MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 37: Optics Alignment (Required For Periodic Inspection Or Installing X-Ray Tube)

    X-ray tube Goniometer Sample axis Alignment Fig. 6.2.1 Optical Alignment Start up MiniFlex 600 (see “ ”). Starting Up the System Open the sample chamber door, and set the included 0.3-mm Cu absorber into the slit box of goniometer arm.
  • Page 38 Attachment and Detector respectively. (See Fig. 6.2.4 and Fig. 6.2.5) Click Goniometer, and set the User setting of Min. to −3°. Update ③ the hardware configuration after the setting is completed. (See Fig. 6.2.6) Fig. 6.2.3 Hardware Configuration window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 39 Optics Alignment (Required for Periodic Inspection or Installing X-Ray Tube) Fig. 6.2.4 Attachment window Fig.6.2.5 Detector window Set to −3゜ Fig. 6.2.6 Goniometer window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 40 Options - Detector Setup – SC-70, and enter 500 mV in the PHA baseline box, 1000 mV in the PHA window box, and the HV value indicated on the label pasted on SC (see Fig. 5.10) in the HV box as the initial value. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 41 The environment for optics alignment has been set up by the above procedures. Adjust the X-ray tube in vertical direction to position the direct beam at an angle of 2θ/θ= 0°. Select Control - Manual Control. ① MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 42 Setting and Adjustment The MiniFlex 600 measures direct beam under the following slit ② conditions. If the intensity of the direct beam is not within the range of 2,000 to 100,000cps, adjust the intensity by changing the number of absorbers or the tube voltage output in DS=1.25°, SS=absorber (Cu 0.3 mm x 1), RS=0.3 mm...
  • Page 43 Peak angle, intensity and FWHM Fig. 6.2.12 Direct beam measurement result (rough adjustment) By clicking the Peak position calculation button, the peak position can be calculated. Specify Full Width at Half Maximum for Peak Search Method. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 44 If the peak position is off to the negative side, turn the tube position ③ vertical adjustment screw in counterclockwise direction (slightly). After the adjustment is completed, tighten the locking screws and perform the measurement of direct beam peak position again by procedures in MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 45 Count mode under Detector: Int. When the direct beam position is within the range of ±0.01°,the tube position adjustment is completed. Fig. 6.2.14 Direct beam measurement conditions (precision measurement) within ±0.01° Fig. 6.2.15 Direct beam measurement result (precision measurement) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 46 Setting and Adjustment In general, correction value is not registered in MiniFlex 600. The angle error can be minimized by setting the “Data Measurement and Setting Procedure for Real-Time 2 theta Axis Correction (Required for Initial Setup or Periodic Inspection)”, which will be described later.
  • Page 47 Click Goniometer, and return the setting of the User setting of Min. ④ to 2°, and update the hardware configuration. The adjustment of SC is completed by the above procedures. To continue the adjustment of D/teX Ultra, go on to Optics alignment (D/teX “ Ultra) ”. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 48: Optics Alignment (D/Tex Ultra)

    Loosen the fixing screws of receiving slit box, and slide the receiving ⑥ slit box to the D/teX Ultra side. Then, tighten the fixing screws. Slide to the D/teX Ultra side Receiving slit box fixing screw Fig. 6.2.18 Moving the receiving slit box MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 49 Fig. 6.2.19 Detector window When performing the optics alignment for the first time after installing the MiniFlex 600, select Options - Detector Setup - D/teX Ultra, and enter the same value as Low value in the PHA baseline box, and High value minus the Low value in the PHA window box as the initial value.
  • Page 50 The correction value is registered in the MiniFlex Guidance automatically after the measurement is completed. Click the OK button. ⑧ The correction value can be seen on the History window. (Click the History command under the View menu to display the History window.) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 51 Soller slits are 2.5°, enter 47.26° in the Theta/2-theta position (deg) box. Click the Execute button. ⑧ The correction value is registered in the MiniFlex Guidance automatically after the measurement is completed. Click the OK button. ⑨ Fig. 6.2.21 D/teX Detector Center Correction window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 52 Setting and Adjustment Enter 0° when using the direct beam Fig. 6.2.22 Measurement condition MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 53 Then, turn the adjustment screw to adjust the height of the beam stop. Perform the procedures in Perform direct beam confirmation ② measurement again, and confirm that the direct beam is blocked by the beam stop. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 54 Adjust the beam stop If an adjustment is required again, return to ⑤ and perform the adjustment. Scan conditions, Absolute, Start: 1, Stop: 5, Step: 0.01, Speed: 10, Scan mode: Continuous Count mode under Detector: Diff. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 55 Optics Alignment (Required for Periodic Inspection or Installing X-Ray Tube) Fig. 6.2.25 Conditions of beam stop position confirmation measurement 3° Fig. 6.2.26 Measurement result of beam stop position confirmation (insufficient adjustment) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 56: Optics Alignment (For D/Tex Only)

    Goniometer Sample axis Alignment D/teX Fig. 6.2.28 Optical Alignment Start up MiniFlex 600 (see “Starting Up the System”). Open the sample chamber door, and set the included 0.3-mm Cu absorber into the soller slit box of the goniometer arm. Make sure that nothing is mounted on the sample holder at this time.
  • Page 57 Click Goniometer, and set the User setting of Min. to −3°. Update ③ the hardware configuration after the setting is completed. Update the hardware configuration after the setting is completed. ④ Fig. 6.2.30 Hardware Configuration window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 58 Setting and Adjustment Fig. 6.2.31 Attachment window Fig. 6.2.32 Detector window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 59 When performing the optics alignment for the first time after installing the MiniFlex 600, select Options - Detector Setup - D/teX Ultra, and enter the same value as Low value in the PHA baseline, and High value minus the Low value in the PHA window box as the initial value.
  • Page 60 Detector Adjustment - D/teX Detector Center Correction. Check the Center Correction Clear checkbox. ② Click the Execute button. ③ Close the window. ④ The environment for optics alignment has been set up by the above procedures. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 61 Adjust the X-ray tube in vertical direction to position the direct beam at an angle of 2θ/θ = 0º. Select Control - Manual Control. ① MiniFlex 600 measures direct beam under the following slit ② conditions. If the intensity of the direct beam is not within the range of 2,000 to ③...
  • Page 62 By clicking the Peak position calculation button, the peak position can be calculated. Specify the Full Width at Half Maximum for the Peak Search Method. When the precision measurement result shows a peak angle within the range of ± 0.01°, the adjustment is completed. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 63 When the direct beam position is within the range of ±0.01°, the tube position adjustment is completed. Scan conditions, Absolute, Start: -0.2, Stop: 0.2, Step: 0.01, Speed: 2, Scan mode: Continuous Count mode under Detector: Int. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 64 (precision measurement) within ±0.01° Fig. 6.2.40 Direct beam measurement result (precision measurement) In general, correction value is not registered in MiniFlex 600. The angle error can be minimized by setting the “Data Measurement and Setting Procedure for Real-Time 2 theta Axis Correction (Required for Initial Setup or Periodic Inspection)”, which will be described later.
  • Page 65 Set DS=1.25° and SS=RS=OPEN. ⑤ When the incident and receiving Soller slits are 5°, enter 47.25°in the Theta/2-theta position (deg) box. When the incident and receiving Soller slits are 2.5°, enter 47.26°in the Theta/2-theta position (deg) box. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 66 ・ If part of or the whole direct beam can be seen, perform the procedures Adjust the beam stop. ・ When it is confirmed that the direct beam is blocked by the beam stop, go on to Perform the beam stop position confirmation measurement. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 67 CAUTION Before performing the beam stop position confirmation measurement, make sure that the direct beam is blocked by the beam stop in Confirm that the direct beam is blocked. The detector may be damaged if the direct beam enters the D/teX Ultra directly. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 68 Scan conditions, Absolute, Start: 1, Stop: 5, Step: 0.01, Speed: 10, Scan mode: Continuous Count mode under Detector: Diff. Fig. 6.2.44 Conditions of beam stop position confirmation measurement 3° Fig. 6.2.45 Measurement result of beam stop position confirmation (insufficient adjustment) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 69 Optics Alignment (Required for Periodic Inspection or Installing X-Ray Tube) 2° Fig. 6.2.46 Measurement result of beam stop position confirmation (adjustment completed) Tighten the beam stop fixing screw and beam stop mounting screw The adjustment of D/teX Ultra is completed by the above procedures. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 70: Hv/Pha Adjustment Of Scintillation Counter (Sc)

    A message confirming whether to register or not will appear after the ③ adjustment is completed. Press the Yes button to register. After the registration is completed, press the OK button to close the ④ window. Fig. 6.3.1 HV/PHA adjustment (SC) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 71 HV/PHA Adjustment of Scintillation Counter (SC) Fig. 6.3.2 Theta/2-theta window Fig. 6.3.3 HV window Fig. 6.3.4 PHA window MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 72 Setting and Adjustment Fig. 6.3.5 Register confirmation message window MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 73: Discriminator Value Setting By D/Tex Ultra

    Set the discriminator value by D/teX Ultra when replacing another D/teX Ultra on the MiniFlex 600 or when performing a measurement for a different wavelength. The discriminator value is specified and differs per individual product, and will not change as long as it is not changed to another individual product.
  • Page 74 Setting and Adjustment Fig. 6.4.1 Adjusting D/teX Ultra Fig. 6.4.2 Adjusting D/teX Ultra Fig. 6.4.3 Register confirmation message window MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 75: Directly Entering The D/Tex Ultra Adjustment Value

    The intensity becomes approximately 60% compared with standard mode. How to calculate from Standard is the following: Fluorescent X-ray Reduce Low = {(Standard Low + Standard High)/2} - 1 MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 76 How to calculate from Standard is the following: Pseudo SC Low = Standard Low +2 Pseudo SC High = Standard High +2 PHA baseline = Pseudo SC Low PHA window = Pseudo SC High - Pseudo SC Low MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 77: Initial Setting Of The Measurement Environment (Required When The X-Ray Tube Type Has Been Changed)

    (Required When the X-Ray Tube Type Has Been Changed) Select Options – Hardware Configuration – X-Ray Generator. Then, select the type of the X-ray tube to be used (target material). Usually, Cu target is used. Fig. 6.5.1 Wavelength table MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 78: Data Measurement And Setting Procedure For Real-Time 2 Theta Axis Correction (Required For Initial Setup Or Periodic Inspection)

    * The sample must be placed evenly and flat. It is important that the sample surface and the sample plate are on the same plane. If it is not so, the angle error margin occurs. The setting jig (with Si) cannot be used for angle correction. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 79 1/7 to 1/10 of FWHM, and the speed needs to be entered so that intensity of each peak is more than 1,500 counts (ideal speed is 10,000 counts). Enter the measurement file name and measurement conditions. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 80 If the X-ray generation is not on, it will start up automatically and the measurement will begin. The measurement time is approximately 80 minutes for SC, and approximately 20 minutes for D/teX Ultra. When the measurement ends, the system automatically calculates and registers the peak position. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 81 (111) are automatically added to the 2θ=0° data. This is based on the fact that, when the low angle error is assumed to be due to the misalignment of the sample surface, the angle error at 0° is approximately close to that of Si (111). MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 83: Startup And Shutdown (Daily Routine)

    HV ENABLE key is stored in a separate place, insert it into the HV ENABLE key hole. Turn on the “Power circuit breaker” on the rear side of MiniFlex 600 main unit (see Fig. 2.2). Then, press the “Power ON switch” on the front side (see Fig.

  • Page 84: Shutting Down The System

    When using tap water, close the faucet of tap water and stop the water from running. If you store the HV ENABLE key in a separate place, remove the key from the panel. The shutting down of MiniFlex 600 is now completed by the procedures above. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 85: Measurement Of Samples (Daily Routine)

    Place a powder paper on top of the sample, and press on the indented section filled with sample with fingertip to compress the sample. Be careful not to move the sample plate during this procedure. MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 86 Powder sample Aluminum sample plate Punch hole (Located on the rear side) Glass plate Sample Glass sample plate Powder paper Measurement surface Fig. 8.1 Preparation of powder sample on aluminum sample plate MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 87: Preparation Of Block Sample On Aluminum Sample Plate

    With this method, halo from the glass or binder is observed and the attached sample is not even. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 88: Cleaning Spilled Or Deposited Powder Sample

    If the powder sample spills from the styrol plastic case or sticks to any other part, vacuum-clean it using a nozzle with a small slit. In addition, wipe it off thoroughly with a piece of cloth or soft paper, wherever it is viable. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 89: Slit System

    Slit system Slit system Regarding the slit conditions, MiniFlex 600 has two types of slit system for measurement: the variable slit system and variable + fixed slit system. The variable slit system enables performing a measurement with the constant irradiation width of 20 mm at the range of 2θ=2～67°. X-ray is irradiated on a measurement while changing the size of the scattering slit along with the sample size 20 mm.
  • Page 90 Sample width is fixed to 20 mm. The sample width of standard sample plate is 20 mm. Set Slit Correction to Enable, and click the OK button. Select the size of DS to be used. Fig. 8.5 Divergence slit correction MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 91: Measurement With Miniflex Guidance

    Condition Setting button. It is convenient to assign a number to a set of typical measurement conditions and specify that number for a routine measurement. Enter File name etc. Measurement Conditions Measurement start button button Fig. 8.6 General Measurement MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 92 SS slit. When using the counter monochromator, remove the Ni filter. Slit condition: Variable + fixed slit system Scan axis: Theta/2-Theta (Fixed) Measurement mode: Continuous Count unit: cps (Changeable at the time of processing.) Start angle: 3° Stop angle: 80° MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 93 (0.030 mm). If Kβ X-ray issues occur with the standard type, use the twice as thick type. Slit condition: Variable + Fixed slit system Scan axis: Theta/2-Theta (Fixed) Measurement mode: Continuous (Fixed) MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 94 Ni filter layered with SS slit. Slit condition: Variable slit system Scan axis: Theta/2-Theta (Fixed) Scan mode: Continuous Counting unit: cps (Changeable at the time of processing.) Start angle: 3° Stop angle: 67° Step: 0.02° Scan speed: 3°/min MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 95 Scan mode: Continuous (Fixed) Counting unit: cps (Changeable at the time of processing.) Start angle: 3° Stop angle: 67° Step: 0.02° Scan speed: 20°/min BG condition: Do not measure (Cannot be used for D/teX Ultra.) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 97: Maintenance

    Turn OFF the “Power circuit breaker” (see Fig. 2.2) on the rear side of the MiniFlex 600 main unit. Wait for at least 30 minutes or more after X-RAY OFF of MiniFlex 600, and then start the replacement procedures. Stop running the cooling water for the X-ray tube.
  • Page 98 Sample chamber X-ray tube door Sample position Tube fixing screws Standard sample holder Tube shield Counter (SC) Fig. 9.2 Inside the enclosure (rear view with the upper cover removed) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 99: Disassembling The X-Ray Tube And Cleaning The Filter

    If the tube flange is hot, the filter may be clogged, resulting in degraded cooling efficiency. Perform maintenance of the X-ray tube by following the procedures below. For maintenance purpose, remove the X-ray tube from MiniFlex 600. Disassemble the X-ray tube. Remove the jetter and then remove the filter.

  • Page 100: Cleaning And Further Information

    The maintenance procedures described above must be performed by the user. For further details technical problems or maintenance contracts, contact the sales representative who you purchased the instrument from as well. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 101: Confirming The Alarm Information

    (Normal condition blue) Description will appear by clicking on the alarm box Fig 9.5 Alarm window Click the alarm box. Description will appear by clicking on an alarm box. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 103: Installing The Optional Sample Attachment

    Installing the Optional Sample Attachment As optional sample attachments, MiniFlex 600 offers a sample rotation attachment and an automatic six sample changer ASC-6AMII (with a sample surface rotation mechanism). The sample rotation attachment is useful for quantitative analysis. By measuring the sample while performing sample surface rotation, it enhances the reproducibility of peak intensity.
  • Page 104 Click Attachment, and select the attachment installed in the Attachment window. Fig. 10.4 Hardware Configuration window Fig. 10.5 Attachment window Click OK in the Attachment window. Click Update in the Hardware Configuration window to save the changes. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 105: Installing The Counter Monochromator (Optional)

    Fig. 11.1 Small diffracted rays deriving from Kβ rays detected with the filter method (Above: Filter method, Below: Monochromator method) Fig. 11.2 Difference in the sensitivity to detect small peaks in data between the filter method (above) and monochromator method (below) MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 106: Installing The Counter Monochromator

    Fig. 11.3 Removing the filter Move the 2θ/θ axis to 90° by Manual control, and then turn OFF the power circuit breaker on the rear side of MiniFlex 600 main unit (see Fig. 2.2). Remove the six screws on both sides of the enclosure, and remove the upper cover of the enclosure from the main unit (see Fig.
  • Page 107 SC to the arm Front Front Fig. 11.4 Removing the SC Install the SC to the monochromator. Monochromator After the SC is assembled SC fixing screws (2) to the monochromator Fig. 11.5 Installing the SC to the monochromator MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 108 Fig. 11.6 Installing the monochromator on the goniometer arm Attach the upper cover of the enclosure. Turn ON the "Power circuit breaker" on the rear side of MiniFlex 600 main unit. Then, press the "power ON switch" on the front side.

  • Page 109: Optics Alignment And Notes On Monochromator

    Si data according to the procedure in “Data Measurement and Setting Procedure for Real-Time 2 theta Axis Correction (Required for Initial Setup or Periodic Inspection)” again after installing the monochromator, and registers the corrected data. MiniFlex 600: Benchtop X-ray Diffractometer...

  • Page 110: Arrangement Of Slits

    Position of receiving slit box (with receiving Soller slit inside) to be Incident Soller slit (inside) beside the monochromator Fig. 11.7 Overall view of optical system Incident cover Position to insert DS and IHS Fig. 11.8 Enlarged image of DS MiniFlex 600: Benchtop X-ray Diffractometer...
  • Page 111 Differential Scanning Calorimeters Specifications Subject to Change without Notice Rigaku Corporation Tokyo Branch 4-14-4, Sendagaya, Shibuya-ku, Tokyo 151-0051, Japan www.rigaku.com Phone: +81-3-3479-0618 Fax: +81-3-3479-6112 e-mail: rinttyo@rigaku.co.jp Rigaku Corporation Rigaku Americas Corporation Rigaku Europe SE Head Office 9009 New Trails Drive,...

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