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MiniFlex 600: Benchtop X-ray Diffractometer

79

Measurement of Samples (Daily routine)

Preparing the Sample Plate

The sample surface which receives the incident X-rays must be flat and
positioned at the rotation center of the goniometer.
Since the surface of the sample plate is machined to be perfectly flat, only
placing the sample plate on the sample holder sets the measurement plane (front
side) of the sample plate at the rotation center of the goniometer.

・

If the sample holder or sample plate is scratched or if dust has adhered to

either, it may result in measurement deviation.

・

It is important to ensure that the sample surface is aligned with the

measurement plane of the sample plate.

・

If the sample surface is concave, the diffracted X-ray shifts toward a lower

angle side. In contrast, a convex sample surface can result in a shift of the
diffracted X-ray toward a higher angle side. In these cases, the deviation in
lower-angles is greater.

Preparation of powder sample on aluminum sample plate

If the sample amount is sufficient, place the sample on the aluminum sample
plate according to the following procedure. (See Fig. 8.1)

1

Hold the sample plate firmly; making sure that the measurement

surface of the sample plate is in contact with the flat glass plate. Then
pour the sample into the indented section of the sample plate.

2

Using the glass sample plate, spread the sample evenly throughout the

indented section.

3

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.

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Содержание MiniFlex 600

Страница 1: ...Benchtop X ray Diffractometer Instruction Manual This image is an example of MiniFlex series The actual product may differ from the image...

Страница 2: ...e results of the use of this manual As a rule one set of the instruction manual has to be purchased for each product If there are any missing or incorrectly collated pages in the delivered instruction...

Страница 3: ...e specifications 11 Standard Software 11 Optional accessories 12 D teX Ultra High speed 1D Detector Optional 12 Installation Condition 13 Installation Room 13 Environmental Conditions of Installation...

Страница 4: ...Environment Required When the X Ray Tube Type Has Been Changed 71 Data Measurement and Setting Procedure for Real Time 2 theta Axis Correction Required for Initial Setup or Periodic Inspection 72 Sta...

Страница 5: ...ple Attachment 97 Installing the Counter Monochromator Optional 99 Installing the Counter Monochromator 100 Optics alignment and notes on monochromator 103 Arrangement of slits 104 Item No 2005L101 L1...

Страница 6: ......

Страница 7: ...ator of 600 W 40 kV 15 mA enables 1 3 times higher output than the existing model The system is a location free tool that can readily be transported and installed in a relatively small indoor or outdo...

Страница 8: ...thus lowers the background and offers data with a higher P B ratio Refer to Installing the Counter Monochromator Optional Although omitted in Fig 1 1 an auxiliary variable DS Divergence slit is place...

Страница 9: ...ion enclosure Enclosure cabinet of the main unit that provides protection from radiation Flow rate detector For monitoring flow rate of cooling water X ray tube LAN cable Computer for Japanese market...

Страница 10: ...t b Block diagram Fig 2 1 Appearance and block diagram of MiniFlex 600 including optional components Heat exchanger Scan HV Detector SC Sample Water cooling Data output 2 X ray X ray tube Electronic c...

Страница 11: ...ew Right side view Rear view Power ON OFF switch OFF ON Sample chamber door LAN cable outport Door knob X Ray warning lamp Power circuit breaker Air vent Emergency off switch EMO Power source inside D...

Страница 12: ...iffractometer Front view perspective drawing Fig 2 3 Major components and names of parts Top view perspective drawing Control driver Beam stop partition to prevent leakage X ray tube Tube shield X ray...

Страница 13: ...Names of Parts MiniFlex 600 Benchtop X ray Diffractometer 7 Fig 2 4 Dimensions of main unit weight approx 80 kg...

Страница 14: ...16 2 17 2 18 Box Aluminum sample plate Glass sample plate 0 2 mm deep Glass sample plate 0 5 mm deep Settingjig withSisample Rectangular glass plate Hex wrench Cu absorber 0 3 mm Al absorber 0 2 mm D...

Страница 15: ...ble through the use of a spring plate X ray shutter Mechanical rotary shutter K filter Ni filter for Cu tube standard thickness 0 015 mm Other filters are optional Goniometer Angle measuring device Ty...

Страница 16: ...T1 Window material Be Effective window diameter 23 mm Dimension 80 mm L Counting control circuit ECP 2 axis minimum step angle 0 01 2 SC high voltage power source 0 to 1000 V Wave height discriminator...

Страница 17: ...op which meets all the specifications described below with Windows 7 Professional 32 bit version installed Main unit CPU Intel Core i3 or later OS Windows 7 Professional 32 bit version Japanese or Eng...

Страница 18: ...database Environmental dust quantitative analysis SiO2 etc software Quantitative analysis software quantitative analysis through the use of the calibration curve method and standard addition method D...

Страница 19: ...l Conditions of Installation Room Vibration of floor The floor must not have vibrations perceivable to the human body Temperature 15 C to 25 C Relative humidity Below 65 no condensation Abrupt changes...

Страница 20: ...1 0 kVA Furnish a 15 A grounded power outlet 3 contact The standard included cable only for Japan is compatible up to 125 V AC For countries outside of Japan it may be required to be prepared by the...

Страница 21: ...mperature 30 C or lower pH 6 5 to 7 5 Electric conductivity 200 cm or less Total hardness 50 ppm or less Silica SiO2 20 ppm or less Iron ion Fe3 0 3 ppm or less Chlorine ion Cl 10 ppm or less Sulfate...

Страница 22: ......

Страница 23: ...sides of the main unit Pull the cover slightly backward and then lift it up Fig 5 1 Removing the upper cover of the enclosure 2 Install the X ray tube Remove the upper cover The X ray tube is on the...

Страница 24: ...ports see Fig 5 3 on the rear side of the main unit Couple the connection ports securely using the included AMC couplings to prevent water leakage 2 Connect the main unit and the cooling water supply...

Страница 25: ...he parts for transportation for SC Fig 5 4b Removing the parts for transportation with beam stop Before installing the SC remove the parts for transportation rotate the balancer of driving motor by ha...

Страница 26: ...meter arm with the two counter fixing screws see Fig 5 6 and Fig 5 9 3 Position of the receiving slit box Check the position of the receiving slit box Loosen the receiving slit box fixing screws and s...

Страница 27: ...cable to the cable joint connector on the SC see Fig 5 8 Fig 5 8 SC Fig 5 9 Assembling the SC A label is attached on the rear side of the SC The HV value indicated on the label will be used as the in...

Страница 28: ...wo receiving slit box fixing screws Fig 5 13 4 Move the receiving slit box so it is positioned right next to the D teX Ultra Fig 5 13 Rotate the balancer of driving motor by hand and move the goniomet...

Страница 29: ...teX Ultra Fig 5 15 SC cable A label is attached on D teX Ultra The discriminator value indicated on the label is used as the Low and High discriminator value Take note and remember these values befor...

Страница 30: ...order to prevent the direct beam from directly entering the D teX Ultra The D teX Ultra may be damaged if the beam stop is not installed Be sure to install the beam stop upon a measurement Installing...

Страница 31: ...d on top of the cam base Fig 5 19 Installing the variable knife edge 3 Align the marker on the sample holder with the marker on the variable knife edge as shown in Fig 5 20 Fig 5 20 Aligning the marke...

Страница 32: ...2 How to release the slider from the retracted position Remove the slider retracting screw while holding the slider of the variable knife edge by hand The slider will slide down when the screw is rem...

Страница 33: ...wer cable connector on the rear side of MiniFlex 600 main unit For power supply input cable with plug single phase 100 V 240 V AC power supply connect the power supply input cable to a dedicated power...

Страница 34: ...stallation Manual ME13445 installation CD of each software is included The MiniFlex Guidance PDXL Basic Software and Integral Intensity Calculation are used for the adjustment of the equipment measure...

Страница 35: ...High resolution Soller inc 2 5deg CAUTION The incident Soller slit cannot be replaced by the user Replacement conducted by the user may cause the system to malfunction Confirming the incident Soller s...

Страница 36: ...s the incident Soller slit is installed When Standard is selected as incident Soller slit the receiving soller slit is 5 0deg When High resolution is selected as incident Soller slit the receiving sol...

Страница 37: ...correct angle Be sure to execute this alignment if an X ray tube is replaced For measurements only by D teX Ultra see Optics alignment for D teX only When 2 0 the DS center sample axis axis center and...

Страница 38: ...bsorber upon an optics alignment 3 Set the environmental settings of goniometer and detector for optics alignment Start up MiniFlex Guidance and select Options Hardware Configuration See Fig 6 2 3 Con...

Страница 39: ...Alignment Required for Periodic Inspection or Installing X Ray Tube MiniFlex 600 Benchtop X ray Diffractometer 33 Fig 6 2 4 Attachment window Fig 6 2 5 Detector window Fig 6 2 6 Goniometer window Set...

Страница 40: ...Set the slit correction to Disable Fig 6 2 7 Angle Correction window Fig 6 2 8 Slit correction window When Manual Control is already opened this change will not be updated to system settings Close the...

Страница 41: ...ame manner select Control Initialize Individual Axis Detector 1 and click the Execute button 7 Select Control XG Control and click the ON button of X Ray Set the tube voltage and tube current to 30 kV...

Страница 42: ...12 cannot be obtained When there are concerns that counting loss such as the top peak becoming flat or being separated into two peaks due to decrease of peak intensity may occur add an absorber or cha...

Страница 43: ...tion Full Width at Half Maximum FWHM Scan conditions Absolute Start 0 4 Stop 0 4 Step 0 01 Speed 5 Scan mode Continuous Count mode under Detector Int Fig 6 2 11 Theta 2 theta axis scan conditions roug...

Страница 44: ...the tube shield Fig 6 2 13 Tube position vertical adjustment mechanism If the peak position is off to the positive side loosen the locking screws and turn the tube position vertical adjustment screw i...

Страница 45: ...Fig 6 2 14 and perform precision measurement of the peak position Scan conditions Absolute Start 0 2 Stop 0 2 Step 0 01 Speed 2 Scan mode Continuous Count mode under Detector Int When the direct beam...

Страница 46: ...with the reflection method measurement The angle error is about 0 003 for 0 01 and correction is unnecessary Initialization procedure Function to move the goniometer to DATUM angle 10 and set that pos...

Страница 47: ...ustment condition Fig 6 2 17 Confirming HV PHA register Select Options Hardware Configuration Click Goniometer and return the setting of the User setting of Min to 2 and update the hardware configurat...

Страница 48: ...g the instructions of Shutting down the system see Shutting Down the System Then remove the radiation enclosure Remove the SC cable from the SC and then remove the SC by the whole SC stage Loosen the...

Страница 49: ...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 T...

Страница 50: ...Center Correction with direct beam Select Tasks Package Measurement Maintenance D teX Detector Adjustment D teX Detector Center Correction Check the Center Correction Clear checkbox Click the Execute...

Страница 51: ...mounted on the variable knife edge remove it Fill the 0 5 mm deep glass sample plate with angle reference material NIST SRM 640d and set it on the sample holder Check the Theta 2 theta scan conditions...

Страница 52: ...Setting and Adjustment 46 MiniFlex 600 Benchtop X ray Diffractometer Fig 6 2 22 Measurement condition Enter 0 when using the direct beam...

Страница 53: ...part of or the whole direct beam can be seen perform the procedures in 8 Adjust the beam stop When it is confirmed that the direct beam is blocked by the beam stop go on to 9 Perform the beam stop po...

Страница 54: ...directly Remove the Cu absorber mounted on Soller slit box Set the setting jig with Si on the sample holder Confirm that the beam stop is not set at a position where it interferes with the measuremen...

Страница 55: ...nspection or Installing X Ray Tube MiniFlex 600 Benchtop X ray Diffractometer 49 Fig 6 2 25 Conditions of beam stop position confirmation measurement Fig 6 2 26 Measurement result of beam stop positio...

Страница 56: ...tra When 2 0 the DS center sample axis axis center and RS center are aligned in a straight line The optics alignment is a procedure to raise or lower the X ray tube in order to move the focus onto thi...

Страница 57: ...tector may be damaged if the absorber is not installed Be sure to install the absorber upon an optics alignment 2 Set the environmental settings of goniometer and detector for optics alignment Start u...

Страница 58: ...Setting and Adjustment 52 MiniFlex 600 Benchtop X ray Diffractometer Fig 6 2 31 Attachment window Fig 6 2 32 Detector window...

Страница 59: ...s 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 The Low value and High value are in...

Страница 60: ...the Execute button When Manual Control is already opened this change will not be updated to system settings Close the Manual Control window and then re open it 5 Clear the D teX Detector Center Correc...

Страница 61: ...e variable DS If the intensity is too strong counting loss dead time occurs and the correct peak shape see Fig 6 2 37 cannot be obtained When there are concerns that counting loss such as the top peak...

Страница 62: ...01 Speed 5 Scan mode Continuous Count mode under Detector Int Fig 6 2 36 Theta 2 theta axis scan conditions rough adjustment stage Fig 6 2 37 Direct beam measurement result rough adjustment By clicki...

Страница 63: ...on slightly If the peak position is off to the negative side turn the tube position vertical adjustment screw in counterclockwise direction slightly After the adjustment is completed tighten the locki...

Страница 64: ...Procedure for Real Time 2 theta Axis Correction Required for Initial Setup or Periodic Inspection which will be described later MiniFlex 600 performs measurement by reflection method measurement of di...

Страница 65: ...ear check box is checked uncheck it Check the Theta 2 theta scan conditions checkbox Set DS 1 25 SS Absorber Cu plate 0 3 mm x 1 or 2 plates and RS OPEN Enter 0 as Theta 2 theta position deg Click the...

Страница 66: ...Soller slit box If the beam stop is not mounted mount it Execute measurement of direct beam and confirm that the direct beam is blocked by the beam stop Scan conditions Absolute Start 0 4 Stop 0 4 St...

Страница 67: ...of the beam stop Perform the procedures in 14 Confirm that the direct beam is blocked again and confirm that the direct beam is blocked by the beam stop Fig 6 2 43 Adjusting the beam stop 16 Perform t...

Страница 68: ...the background intensity at 2 2 or larger is not blocked by the beam stop If an adjustment is required again return to 15 Adjust the beam stop and perform the adjustment Scan conditions Absolute Start...

Страница 69: ...ube MiniFlex 600 Benchtop X ray Diffractometer 63 Fig 6 2 46 Measurement result of beam stop position confirmation adjustment completed 17 Tighten the beam stop fixing screw and beam stop mounting scr...

Страница 70: ...cause the pulse to not pass the PHA This is the same with when the X ray tube target is changed Readjustment of HV and PHA of the SC is necessary to let the characteristic X ray pass the PHA efficien...

Страница 71: ...HV PHAAdjustment of Scintillation Counter SC MiniFlex 600 Benchtop X ray Diffractometer 65 Fig 6 3 2 Theta 2 theta window Fig 6 3 3 HV window Fig 6 3 4 PHA window...

Страница 72: ...Setting and Adjustment 66 MiniFlex 600 Benchtop X ray Diffractometer Fig 6 3 5 Register confirmation message window...

Страница 73: ...g the value of the D teX Ultra s discriminator compared with SC reduces the effect of fluorescent X rays or improves intensity by lowering the wavelength separation resolution and obtaining peripheral...

Страница 74: ...Setting and Adjustment 68 MiniFlex 600 Benchtop X ray Diffractometer Fig 6 4 1 Adjusting D teX Ultra Fig 6 4 2 Adjusting D teX Ultra Fig 6 4 3 Register confirmation message window...

Страница 75: ...n and intensity of D teX Ultra It is set to take in the wavelength area in which the diffracted X ray intensity is 10 or higher which is mainly the used wavelength The two values written on the label...

Страница 76: ...nt X ray Reduce Low Pseudo SC A setting to take in 2 extra channels high energy side and low energy side compared with standard mode Intensity increases compared with Standard but becomes more easily...

Страница 77: ...600 Benchtop X ray Diffractometer 71 Initial Setting of the Measurement Environment Required When the X Ray Tube Type Has Been Changed Select Options Hardware Configuration X Ray Generator Then select...

Страница 78: ...o a level equivalent to the angle reproducibility of goniometer This makes the system independent from the mechanical accuracy of the goniometer The impact of the differences between individual goniom...

Страница 79: ...nd measurement conditions If the items in Optics element conditions are changed click the Default button The reference conditions will be automatically entered in Peak measurement conditions If user w...

Страница 80: ...dard sample holder Fig 6 6 3 Standard sample holder and glass sample plate 5 Click the Execute button and execute the measurement If the X ray generation is not on it will start up automatically and t...

Страница 81: ...Check whether an angle difference between the input measured value and the logical value exceeds the range of 0 1 Under normal conditions the difference does not exceed the range of 0 1 8 By selectin...

Страница 82: ......

Страница 83: ...ON switch on the front side see Fig 7 1 to turn on the power of the equipment 3 The Door Lock button will blink Press the Door Lock button The door is locked Fig 7 1 Names of panel switches and front...

Страница 84: ...warning lamp on top of the enclosure will turn off 2 End MiniFlex Guidance Each window can be left open 3 Shut down the PC 4 Wait at least 3 or more minutes after the X ray generation has stopped and...

Страница 85: ...ace is concave the diffracted X ray shifts toward a lower angle side In contrast a convex sample surface can result in a shift of the diffracted X ray toward a higher angle side In these cases the dev...

Страница 86: ...ed section when the sample plate is raised The measurement surface of the aluminum sample plate is the rear side with which the glass plate was in contact Fig 8 1 Preparation of powder sample on alumi...

Страница 87: ...han the Al sample plate If the sample amount is sufficient pour the sample on the indented section of the glass sample plate and spread the sample evenly using another glass sample plate so the sample...

Страница 88: ...glass plate Keep in mind that if the sample amount is small the intensity of diffracted X rays will appear lower in the high angle area thus reducing the reliability of results A binder is usually pr...

Страница 89: ...o 145 respectively in a measurement By using slit correction the intensity of the variable slit used at the low angle side can be corrected to the intensity of fixed slit Slit Correction The irradiati...

Страница 90: ...lex 600 Benchtop X ray Diffractometer 2 Sample width is fixed to 20 mm The sample width of standard sample plate is 20 mm 3 Set Slit Correction to Enable and click the OK button Select the size of DS...

Страница 91: ...menu of MiniFlex Guidance 1 Select Package Measurement General Measurement In this window specify the names of the folder and file where you want to save measurement data and the name of the sample T...

Страница 92: ...n Counter as the detector are as follows Enter the measurement conditions by using these conditions as a reference X ray 30 kV 15 mA 40 kV 15 mA if counter monochromator is used Slit DS 1 25 and 10 mm...

Страница 93: ...not appear The conditions for qualitative analysis data measurement when using D teX Ultra as the detector are as follows Enter the measurement conditions by using these conditions as a reference X ra...

Страница 94: ...s end Under the Specification B X ray generation does not need to be turned off when opening the door It is therefore not necessarily required to set the equipment to turn off X ray generation after m...

Страница 95: ...cattering slit SS OPEN Receiving slit RS OPEN Insert the Ni filter into the position of the receiving slit There are two types of Ni filter standard type 0 015 mm and twice as thick type 0 030 mm If K...

Страница 96: ......

Страница 97: ...ll the X ray tube at times such as when it is necessary to replace the X ray tube or to clean the filter of the jetter of the X ray tube Tools used Philips screwdriver slotted screwdriver waste cloth...

Страница 98: ...two screws of X ray tube Tool used Slotted screwdriver 6 Remove the X ray tube CAUTION Make sure that the water remaining inside the X ray tube does not drip inside the tube shield If the water drips...

Страница 99: ...ing water hose 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 b...

Страница 100: ...allowed To prevent this risk observe the following precautions avoid contact with any part of the body and do not moisten polish chip or cut beryllium Cleaning and Further Information If the sample is...

Страница 101: ...information can be confirmed in MiniFlex Guidance by the following procedures 1 Start up MiniFlex Guidance and select Control XG control The XG Control window appears Fig 9 4 XG Control window 2 Click...

Страница 102: ......

Страница 103: ...tative analysis as well To use any of these optional sample attachments install it on the standard sample holder This section describes how to install the 6 sample changer on the standard sample holde...

Страница 104: ...ay Diffractometer 5 Click Attachment and select the attachment installed in the Attachment window Fig 10 4 Hardware Configuration window Fig 10 5 Attachment window 6 Click OK in the Attachment window...

Страница 105: ...with a Cu tube To solve these problems a counter monochromator dedicated for Cu tube is offered as an option It is an optical system which disperses a beam by means of a graphite crystal and only cou...

Страница 106: ...er monochromator is described below 1 Set the setting jig Si plate on the sample holder Remove the filter and perform measurement to obtain the intensity of Si 111 By comparing the intensity without m...

Страница 107: ...spacer from the SC see Fig 11 4 Fig 11 4 Removing the SC 5 Install the SC to the monochromator Fig 11 5 Installing the SC to the monochromator SC Monochromator SC fixing screws 2 After the SC is assem...

Страница 108: ...slit box is positioned besides the monochromator Fig 11 6 Installing the monochromator on the goniometer arm 7 Attach the upper cover of the enclosure 8 Turn ON the Power circuit breaker on the rear...

Страница 109: ...X ray intensity is too strong at 30 kV 10 mA decrease to 26 kV 10 mA The X ray intensity will become approx 1 14 when a single Al 0 2 mm plate is added Adjust the optical system according to the same...

Страница 110: ...ts Fig 11 7 Overall view of optical system Fig 11 8 Enlarged image of DS Position to insert DS and IHS Incident cover Variable DS inside Sample holder X ray tube DS SS RS SC Monochromator Position of...

Страница 111: ...oration Rigaku Americas Corporation Rigaku Europe SE Head Office 3 9 12 Matsubara cho Akishima shi Tokyo 196 8666 Japan Phone 81 42 545 8189 Fax 81 42 544 9223 e mail rinttyo rigaku co jp 9009 New Tra...

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