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XRD Laboratory Mineralogy Analyser

Benchtop XRD/XRF for Laboratories

The Next Generation in X-ray Diffraction Instrumentation Laboratory Powder X-ray Diffractometer (PXRD)

Initially conceived to perform chemical and mineralogical testing for NASA’s Mars Science Laboratory (MSL) miss

ion, the BTX is a self-contained benchtop instrument which harnesses advanced dual XRD/XRF technology and renders it for earthbound applications. Combining both Olympus and NASA innovation, BTX brings to life a new way of performing X-ray diffraction and X-ray fluorescence measurements.

Using a specifically developed direct excitation charge coupled device (CCD) “camera”, BTX is able to collect X-ray photon data for both X-ray diffraction and X-ray fluorescence simultaneously. This is the result of the integrated camera’s ability to detect both photon position and photon energy at the same time. With energy resolution of -200 eV (5.9 keV), BTX makes XRF analysis as simple as viewing the software spectrum display.



Selecting Your X-ray Source: Cobalt Vs. Copperxrd laboratory mineralogy analyser (1)

Olympus XRD (X-ray Diffraction) instruments come equipped with either a copper (Cu) or cobalt (Co) X-ray tube. For most applications the same performance for compound identification is achieved with either a Cu or Co tube, however, for best results some applications are more suitable for one or the other.

Several key factors differentiate between the two X-ray tube options to help determine which X-ray source will give the best performance for a specific application. Clearly distinguishable peaks provide the most accurate compound identification. For some applications with specific sample matrices, the X-ray tube can help in optimizing the diffraction peak-to-noise ratio or the visibility of the diffraction peaks.

Optimizing Peak-to-Noise Ratio

A high peak-to-noise ratio enables accurate identification of the XRD pattern. Two of the phenomena that can affect this ratio are secondary fluorescence and absorption, which occur as a function of the energy of the X-rays and of the major elements composition of the sample. The choice of tube will influence both absorption and secondary fluorescence so it is important to consider these two effects when choosing your tube. For instance, high Fe/Co- containing samples will strongly absorb and fluoresce under Cu radiation, while high Mn/Ti/Ca-containing samples will strongly absorb and fluoresce under Co radiation.


Absorption is caused when incoming X-rays get absorbed by the elements in the sample and do not get the chance to diffract. This results in lower diffraction peak intensity and therefore, a lower peak-to-noise ratio.

Secondary fluorescence occurs when incoming X-rays excite core electrons from specific elements present in the sample causing increased background and therefore, a lower peak- to-noise ratio. The Olympus Smart Sense filter compensates for this occurrence by filtering out some amount of the counts that have a different energy than the X-ray source although it simultaneously decreases the overall X-ray signal.



Optimizing Peak Shift

The XRD fingerprint is specific to each compound. Some compounds have critical identifying peaks that show up at very low angles or very high angles. The choice of Cu or Co tube has two effects on the peak placement within our detector’s visible range of 5 – 55° 20: shift in the 20 range and compression/expansion of the pattern. The right tube choice will result in the optimum shift to see the peaks of interest for a particular substance.

A Cu tube compresses the XRD pattern and shifts to low angles as compared to Co. As a result, a wider range of diffraction peaks become visible and more XRD information for compound identification can be collected but there can be a tradeoff in resolution caused by the compression of the pattern, which can result in peak overlap.

A Co tube shifts the XRD pattern towards high angles, increasing the visibility of low angle peaks. The diffraction peak information collected at low angles is especially important for clay minerals typically showing an intense peak at low angle, but there can be a tradeoff in missing diffraction peaks at high angles.

Quartz Sample Measured With a Co and With a Cu Tube


For applications with sample matrices affected by the X-ray tube, the choice between a Cu and Co is a matter of balancing the various effects such as the ones described in this document. The Olympus team of application scientists is available to assist with XRD instrument selection and configuration for your specific application needs to achieve the best possible results.


Easy Sample Preparation

BTX radically simplifies sample collection and preparation for your X-ray diffraction experiments. Typically, a sample must be finely ground and pressed into a pellet in order to ensure a sufficiently random orientation of the crystals.

BTX’s patented sample vibration chamber eliminates that issue. Requiring a mere 15 mg sample, the vibration chamber’s convection process presents the instrument optics with multifarious orientations of the crystalline structure. This results in a superb X-ray diffraction pattern, virtually free of problematic preferred-orientation effects encountered when using classic preparation methods.

Due to its unique powder handling system, nonmechanical goniometers, and lack of complicated moving parts, BTX is able to provide full laboratory-grade powder XRD performance at a fraction of the price.




XPowder Software

BTX is shipped with the necessary software (XPowder) for processing the resulting X-ray diffraction data. This includes the AMSCD mineral database. Should the user wish, XPowder provides the ability to use the ICDD Powder Diffraction Files (PDF).

For quantitative analysis, XPowder comes complete with reference intensity ratio (RIR) quantitative analysis methods as well as full-pattern analysis tools.

Furthermore, BTX provides XRD pattern data in a variety of file formats, making XRD pattern interpretation in third-party programs easily accessible.



BTX operates off software embedded in the unit itself. The user accesses the operating system through an Ethernet or a wireless connection (802.11b/g). This remote operation method allows for a wide degree of flexibility in controlling the instrument and subsequent data handling.



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XRD Analyser Safety

Label and Symbols

Safety-related labels and symbols are attached to the BTX II X-ray Diffraction Analyzer at the locations shown in Figure i-1 on page 1. If any of the labels or symbols are missing or illegible (see Figure i-2 on page 1), please contact Olympus.



The rating plate label is located on the back of the BTX II (see Figure i-3 on page 2). The contents of the label are described in Table 1 on page 2.



Important Information — Please Read Before Use

Intended Use

The BTX II X-ray Diffraction Analyzer is designed primarily for analyzing a variety of powder sample types.

Do not use the BTX II 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 essential information on how to use this Olympus product safely and effectively. Before using this product, thoroughly review this instruction manual, and use the product as instructed.

Keep this instruction manual in a safe, accessible location.

System Compatibility

Do not use incompatible equipment with the system

Using incompatible equipment could cause malfunction and/or equipment damage.

Repair and Modification

The BTX II does  not contain any user-serviceable parts.

In order to prevent human injury and/or equipment damage, do not disassemble modify, or attempt to repair the system.

Safety Symbols

The following safety symbols might appear on the system and in the instruction manual:


General warning symbol:

This symbol is used to alert the user to potential hazard. Obey all safety messages that follow this symbol to avoid possible harm.


Radiation warning symbol:

This symbol is used to alert the user to the presence of potentially harmful ionizing radiation generated within the system. Obey all safety messages that follow this symbol to avoid possible harm.


High voltage warning symbol:

This symbol is used to alert the user to potential electric shock hazards greater than 1000 volts. Obey all safety messages that follow this symbol to avoid possible harm.

Safety Signal Words

The following safety symbol might appear in the documentation of the system:


The DANGER signal word indicates an imminently hazardous situation. It calls attention to a procedure, practice, or the like, which, if not correctly performed or adhered to will result in death or serious personal injury. Do not proceed beyond a DANGER signal word until the indicated conditions are fully understood and met.


The WARNING signal word indicates a potentially hazardous situation. It calls attention to a procedure, practice, or the like, which, if not correctly performed or adhered to could result in death or serious personal injury. Do not proceed beyond a WARNING signal word until the indicated conditions are fully understood and met.


The CAUTION signal word indicates a potentially hazardous situation. It calls attention to an operating procedure, practice, or the like, which, if not correctly performed or adhered to, may result in minor or moderate personal injury, material damage, particularly to the product destruction of part or all of the product, or loss of data. Do not proceed beyond a CAUTION signal word until the indicated conditions arc fully understood and met.

Note Signal Words

The following safety symbols could appear in the documentation of the system:


The IMPORTANT signal word calls attention to a note that provides important information, or information essential to the completion of a task.


The NOTE signal word calls attention to an operating procedure, practice, or the like, which requires special attention. A note also denotes related parenthetical information that is useful, but not imperative.


The TIP signal word calls attention to a type of note that helps you apply the techniques and procedures described in the manual to your specific needs, or provides hints on how to effectively use the capabilities of the product.


Before turning on the system, verify that the correct safety precautions have been taken (see the following warnings). In addition, note the external markings on the system, which are described under Safety Symbols.


General Warnings

  • Carefully read the instructions contained in this instruction manual before turning on the system.
  • Keep this instruction manual in a safe place for further reference.
  • Follow the installation and operation procedures.
  • It is imperative to respect the safety warnings on the system 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 not perform any unauthorized modification to the system.
  • Service instructions, when applicable, are for trained service personnel. To avoid the risk of electric shock, do not perform any work on the system unless qualified to do so. For any problem or question regarding this system, contact Olympus or an authorized Olympus representative.


Radiation Safety Warning

Do not open the system, disassemble, or modify any internal components. These actions could result in serious damage to the system and a health hazard to the operator.


  • The mains plug shall only be inserted into a socket outlet provided with a protective earth contact. Never negate this protective action by using an extension cord (power cable) without a protective conductor (grounding).
  • If there is any possibility that the ground protection could be impaired, you must make the system inoperative and secure it against any unintended operation.
  • The system must only be connected to a power source corresponding to the type indicated on the rating plate.


High Voltage

The BTX II uses a 30 kV high-voltage power supply (HVPS) for X-ray generation. The permanent connection between the HVPS and the X-ray tube is sealed and shielded in such a way that no high voltage connector could accidentally get loose or disconnected inside the system. There is no high voltage risk to the user when using BTX II under normal conditions. Should you notice substantial damage to the outside of the system, or suspect any internal damage after excessive shock, DO NOT turn on the system, return it to the factory for full inspection and potential repairs.


  • X-ray tubes and detectors in this instrument contain beryllium metal in the form of coated foil. In its as-supplied state, the beryllium poses no harm to the user. However, if a detector or tube is damaged, contact with small particles is possible if the instrument is breached (e.g. window broken or during window replacement). Intact skin is sufficient protection against this situation and washing with soap and water will effectively remove any beryllium contamination. If granulated beryllium imbeds in an open wound, seek medical attention.
  • Instruments where the detector or tube is damaged must be returned to your local distributor or the manufacture. Care should be taken to limit the release of beryllium from the instrument

EMC Directive Compliance

FCC (USA) Compliance

This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to Part 15 of the Federal Communications Commission (FCC) rules. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses, and can radiate radio frequency energy, and if not installed and used in accordance with the instruction manual, might cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference, in which case you will be required to correct the interference at your own expense.

ICES-001 (Canada) Compliance

This Class A digital apparatus complies with Canadian ICES-001.

Cet appareil numerique de la classe A est conforme a la norme NMB-001 du Canada.

Before operating your system, you must read, understand and comply with the regulations as detailed in the HC Radiation Emitting Devices (RED) regulation. Details on the regulations relevant to analytical x-ray producing devices, such as the Olympus BTX II can be found at:

US Compliance

The Olympus BTX II X-ray Diffraction Analyzer is compliant with US FDA CFR 1020.40. This regulation mandates radiation protection safety systems, and ensures the product is not hazardous for routine operation. US FDA CFR 1020.40 specifically details that “the provisions of this section are not applicable to systems which are designed exclusively for microscopic examination of material, for example, X-ray diffraction, spectroscopic, and electron microscope equipment or to systems for intentional exposure of humans to X-rays.” Olympus abides by this section in an effort to take all reasonable steps to eliminate radiation exposure to operators.

Before operating your system, you must read, understand and comply with the regulations as appropriate for your state. Contact your state department of public health, radiation protection, for the specific guidelines associated with the operation of a “minimal threat” device such as the Olympus BTX II product.

CE (European Community)

EN 61010-1: Safety requirements for electrical equipment for measurement, control and laboratory use – Part 1: General requirements (1EC 61010-1:2001):

EN 61326-2006: Electrical equipment for measurement, control and laboratory use – EMC requirements (IEC 61326-1:1997 + IEC 61326-1/A1:1998 + IEC 61326-1/A2:2000 + Annexes E and F of IEC 61326:2002 + Corrigendum:2002);


Warranty Information

Olympus guarantees your Olympus product to be free from defects in materials and workmanship for a period of one year. The Olympus warranty only covers equipment that has been used in a proper manner, as described in this instruction manual, and that has not been subjected to excessive abuse, attempted unauthorized repair, or modification.

Inspect materials thoroughly on receipt for evidence of external or internal damage that might have occurred during shipment. Immediately notify the earner making the delivery of any damage, because the carrier is normally liable for damage during shipment. Retain packing materials, waybills, and other shipping documentation needed in order to file a damage claim. After notifying the carrier, contact Olympus for assistance with the damage claim and equipment replacement if necessary.

This instruction manual explains the proper operation of your Olympus product. The information contained herein is intended solely as a teaching aid and shall not be used in any particular application without independent testing and for verification by the operator or the supervisor. Such independent verification of procedures becomes increasingly important as the criticality of the application increases. For this reason, Olympus makes no warranty, expressed or implied, that the techniques, examples, or procedures described herein are consistent with industry standards, nor that they meet the requirements of any particular application.

Olympus reserves the right to modify any product without incurring the responsibility for modifying previously manufactured products.

Technical Support

Olympus is firmly committed to providing the highest level of customer service and product support. If you experience any difficulties when using our product, or if it fails to operate as described in the documentation, first consult the user’s manual, and then, if you are still in need of assistance, contact our After-Sales Service. To locate the nearest service center, visit the Service Centers page at:

BTX II X-ray Diffraction Analyzer Overview

The Olympus BTX II is a benchtop XRD/XRF (X-ray diffraction / X-ray fluorescence) system designed primarily for analyzing a variety of powder sample types. Phase identification is obtained by comparing the diffraction signature of a sample with a database of XRD mineral patterns. The addition of XRF allows easy screening during the phase identification process and can alleviate rare uncertainties.

The BTX II uses a low power X-ray source and 2-D charge coupled device (CCD) detector to obtain XRD data, and a low power X-ray source and a silicon drift detector (SDD) to obtain XRF data. Single minerals or simple mixtures are typically identified after just a few minutes of integration.

The BTX II incorporates the following independent safety protection circuits:

  • Power key switch — Key must be inserted and in the ON position to turn the system on.
  • X-ray warning indicators — LEDs on the front panel illuminate when X-rays are being generated, and also during the power on sequence.
  • Sample carrier safety interlock — High voltage from the power supply is interrupted and generation of X-rays ceases if the sample carrier is removed during system operation.

Packing List

The following table lists the BTX II X-ray Diffraction Analyzer components (see Table 3 on page 10).

xrd analyser btx ii x-ray diffraction analyzer components

xrd analyser btx ii x-ray diffraction analyzer components continued

Front/Top Panel

The front and top panels are where all BTX II controls, indicators, and the sample chamber are located (see Figure 1-1 on page 12 and Table 4 on page 12).



Power Key Switch

Turn the power key clockwise to turn the BTX II on (see Figure 1-2 page 12).


Sample Chamber

The sample chamber is located in the center of the top panel. The clamp lever locks and unlocks the sample carrier (see figure 1-3 on page 13).



The keypad allows you to make selections on the main display to set up and run tests, and save results (see Figure 1-4 on page 13).


Stop/Emergency Shutoff Button

The Stop/Emergency Shutoff button allows you to stop an in-progress test, turn off system power in an emergency, or cancel a selection when using the keypad and main menu to set up tests (see Figure 1-5 on page 13).



The display shows selections for setting up and monitoring tests (see Figure 1-6 on page 14).


LED Indicators

The LED indicators show the status of the high-voltage power supply. X-ray tube, and safety interlocks (see Figure 1-7 on page 14).


Rear Panel

The rear panel is where all BTX II connectors are located (see Figure 1-8 on page 14 and Table 5 on page 15).



Safety Information

This chapter contains important safety information for using the BTX II X-ray Diffraction Analyzer.

Radiation Safety Information

The fundamental principle in radiation protection is that all radiation exposures should be maintained as low as reasonably achievable (ALARA). This is referred to as the ALARA principle. The three key factors which influence an individuals radiation dose from a given source are time, distance and shielding. Control of these factors is the key to keeping the radiation 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 be reduced by the same fraction.
  • Distance
    Distance can effectively reduce a radiation done. When the working distance from the radiation source is increased by a factor of two, the dose received from that source is reduced by a factor of four. This is referred to as the inverse square law, i.e., the radiation intensity from a point source decreases by the square of the distance from the source.
  • Shielding
    Shielding is any material used to reduce the intensity of radiation by absorbing or attenuating the radiation coming from the source.


Do not open the system, disassemble, or modify any internal components. These actions could result in serious damage to the system and a health hazard to the operator.

Safety Interlocks

The BTX II uses an X-ray tube that produces ionizing radiation up to 30 keV at very low power (10 W) as compared to laboratory XRD systems (typically greater than 1 kW). The BTX II system is designed with internal X-ray shielding to fully protect operators and internal components.

The radiation producing components are completely contained within 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 for any BTX II operator to bypass any radiation safety switches. The BTX II fully complies with the FDA CFR, section 1020.40 including safety interlocks and radiation measurements. The BTX II has no measurable radiation leakage from any surface during operation. This is because of the shielding of the X-ray generation and detection components, and the low operating potential and power of the X-ray generation source.

The BTX II incorporates several independent safety interlock circuits to protect the operator. See Figure 2-1 on page 18 and Table 6 on page 18.

xrd-analyser-btx-ii-radiation safety features

xrd-analyser-safety features

Figure 2-2 on page 19 shows the LEDs described in Table 7 on page 20. Table 7 describes the behavior of the LEDs in relation to X-ray emissions.



a. A current drop during a measurement can be related to a filament failure. In such a case, please contact the Olympus After-Sales Service. If the filament fails, the X-ray automatically turns off while the high voltage remains active. The X-ray tube is specifically designed to withstand such a breakdown and the electrical safety is maintained.

Radiation Dose Measurements

Radiation dose measurements were made to document any possible ionizing radiation dose to a typical operator of the BTX II. The measurements were made using a calibrated Ludlum Model 9-3 Radiation Ion Chamber. This chamber is capable of measuring low energy X-ray fields to within plus or minus 20 % of true value above 10 keV, with a typical counting range of 0 to 200 mR/hr.

During testing, the BTX II X-ray Diffraction Analyzer was operated at X-ray tube conditions which are standard for all testing materials (30 kV, 330 µA). Radiation dose measurements were made at specific locations at the base, back, front, and sides of the system.

Radiation dose measurements around the perimeter of the system, at a distance of less than 2 cm, yielded no measurable radiation levels (less than 0.2 mR/hr). 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 dosage to the general public of naturally occurring sources of ionizing radiation.

Figure 2-3 on page 21 shows the radiation dose measurement points. The radiation levels measured at these points are reported in Table 8 on page 21. All measurements were made at maximum 30 kV, 330 µA power setting.



XRD Analyser Operations

Setting Up and Operating the BTXII X-ray Diffraction Analyzer

This chapter provides information for turning ON and OFF the BTX II X-ray Diffraction Analyzer, preparing samples, and testing samples.

Connecting AC power to the BTX II

You power the BTX II by connecting AC power.

To connect AC power

  1. Plug the power supply output cord into the rear panel External Power connector. Push the plug down, and then turn clockwise until the lock ring snaps into place (see Figure 3-1 on page 23).
  2. Plug one end of the AC power cord firmly into the power supply.
  3. Plug the other end of the power cord into a live AC (mains) power outlet.

Turning On or Off the BTXII

To turn on the BTX II

  • Turn the Power Key clockwise to the ON position (see Figure 1-2 on page 12).
    The system briefly displays the message:
    Welcome to BTX II!—Booting
    Please wait
    After about a minute, the display reads:
    Cooling to: -45
    Current temp: (temperature)
    After the detector cools to -45 °C, the main menu appears.

To turn off the BTXII in an emergency situation

  • Turn the Main Power key switch to OFF.
    Press the Stop/Emergency Shutoff button twice (quickly).

To turn off the BTX II under normal conditions

  1. Select Shut Down from the main menu to power the unit off.
    The display reads:
    Shutting down
    Please wait
  2. After the unit is off, turn the main power key switch to OFF.

Preparing a Sample for Analysis

BTX II is designed to operate with coarsely ground samples. The samples must be dry and be able to pass through a 150 µm sieve. Also the sample size should be large enough to convect within the sample cell. Very small particles generally do not perform well within a standard BTX II sample cell. The particles tend to stick to one another and not convect as they should. If you encounter this condition, contact Olympus for details on either increasing the sample cell volume, or to purchase an alternate sample cell.

To prepare a sample

  1. Crush the sample in a crusher (see Figure 3-2 on page 24).
    The result is a sample with a variety of particle sizes.


2. Refine the sample further using a sample sieve (see figure 3-3 on Page 25).


Loading a Sample Into the Sample Cell

There are three components of a BTX II sample cell (see Figure 3-4 on page 25):

  • 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 inner and outer cell.
  • An outer cell window that is similar to the inner cell window, but without a notch at the top.

The BTX II has a cell carrier that can accommodate two cell assemblies. Only side A should be used when loading a cell. Side B is provided as a counter mass for vibration and as a spare cell (see Figure 3-4 on page 25).


The BTX II is supplied with an external shaker assembly to ease sample loading and unloading. The external shaker assembly is used in conjunction with the sample cell to “shake” or vibrate the sample into the cell assembly.

To load a sample into a sample cell

  1. Connect the external shaker plug to the external shaker connector on the main console (see Figure 3-5 on Page 26).


2. Insert the sample carrier into the external shaker and gradually load a small amount of material (enough to fill the gap created by spacer) into the cell assembly side A. The material should be approximately 50 mg of coarsely ground (100-150 µm) powder.


3. In the main display, select Shake, then press the Check button.

4. Adjust the shaking amplitude using the Left arrow and Right arrow buttons.

5. To save the selected shaking amplitude value, press the Check button.

6. When the cell appears to be full, press the Stop button, and then remove the sample carrier from the external shaker.

Testing Sample

To test a sample

  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 3-7 on Page 27).


2. Lock the sample carrier in place by pushing the lever down (see Figure 3-8 on page 27)


3. Select Start acquisition in the main display, then select a running mode (see Table 9 on page 28).


4. Press the Check button to start the test.

When the test begins, the BTX II gives the data set a name based on a sequential number. The red LEDs glow, indicating high voltage to the X-ray tube. The main display shows the voltage and intensity readings, and the sample carrier emits a high-pitched vibration noise.

To stop testing before all the exposures are taken

  • Press the Stop button once.

Unloading a Sample

To remove the sample carrier from the sample chamber

  1. Lift the lever to unlock the sample carrier.
  2. Lift the sample 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.
    1. Using a 1.5 mm hex driver, carefully remove the holding screws, and then disassemble the cell windows and spacer (see Figure 3-9 on page 29).
    2. Clean or replace the cell parts as necessary.


To reassemble a cell

  1. Lay the notched inner window down first (see Figure 3-10 on page 29). Make sure the polymer film faces up.
  2. Place the spacer on top of the inner window.
  3. Place the outer window on top of the spacer.
    Make sure the polymer film faces the spacer.


4. Align the windows and spacer so that the holes in the cell assembly are aligned with the holes in the sample carrier (see Figure 3-11 on page 30).
5. Replace the holding screws, being very careful not to puncture the polymer window material.
6. Tighten the holding screws.


BTX II Software User Interface

This chapter provides information on using the BTX II software user interface. The software user interface allows access to all the features of the system. The software runs in a web browser of your choice. You can connect to the BTX II software user interface over a Wi-Fi or ethernet connection.

Connecting Your Wi-Fi Enabled Device to the BTX II

Establishing a wireless connection requires a Wi-Fi enabled device with a compliant 802.1 lb/g/n connection. This can be a PC, tablet, or other device. When operating, the BTX II broadcasts an unsecured network identified by the serial number of the unit. For example, if the serial number of your BTX II is “002”, then it broadcasts on a network identified as “BTX-002”.

To access the BTX II software user interface

  1. Connect to your network using the standard wireless protocol provided with your Wi-Fi enabled device (see Figure 4-1 on page 31).
    Connecting to the BTX II does not require a password.


2. Start a web browser on your device.

3. Point the browser to the IP address: http://192.168-0.222.
This initiates a connection with the BTX II software user interface.

Connecting the BTX II to Your Ethernet Network

To connect the BTX II to your Ethernet network

  1. Make sure an ethernet cable is connected to the Ethernet connector on the rear of the BTX II.
  2. Make sure the BTX II is on and the Main menu is displayed (See Figure 4-2 on page 32).
  3. Press both the Left arrow and Right arrow buttons at the same time to display the Advanced menu (See figure 4-3 on page 32).
  4. Press the Down arrow button to select Configure Network (See Figure 4-4 on page 32).
  5. Press the Check button to confirm the selection and move to the DHCP (Dynamic Host Configuration Protocol) menu (See Figure 4-5 on Page 33).
    Your LAN must be capable of connecting using DHCP. If your network does not recognize DHCP, contact your IT department for the proper addresses.
  6. Use the arrow buttons to set WIRED to ON.
    Use the left or right arrow button to move to the previous or next fields.
    Use the up or down arrow button to change the value or setting in the current field.
  7. To quickly set up the protocol, use the arrow buttons to set DHCP to ON. Otherwise, change the DHCP parameters using the arrow buttons.
  8. Press the Check button to accept the changes and restart the BTX II.
    The BTX II restarts with the new DHCP configuration.
  9. Navigate back through Main Menu > Advanced Menu > Configure Network > DHCP Menu to view the network-assigned IP address: see procedure ‘To connect the BTX II to your Ethernet network” on page 32, steps 2 through 5.


The network-assigned IP address must be used in your Web browser to access the BTX II software. The default IP address ( is invalid once the network assigns an IP address.

Using the Software User Interface

The BTX II software user interface is accessed through three tabs:

  • Status
  • Data
  • Settings
    (Help is unavailable in the current software release)

Status Tab

The Status tab displays real-time information from the BTX II. You can also control data acquisition using the Start button to initiate an analysis, and the Stop button to end the acquisition sequence (see Figure 4-6 on page 34).


Data Tab

The Data tab has three sub-tabs:


Displays the current XRD two-theta scan, or diffractogram. Note that the screen updates with each new exposure. The screen markers are reference markers for standard reference samples. The markers are: Quartz = green. Beryl = blue (see Figure 4-7 on page 35).



The XRF tab displays the current XRF spectrum calibrated in keV. Routine element markers are identified on the display. This screen updates with each new acquisition (see Figure 4-8 on page 35).



The Files tab allow you to download result files from the BTX II to your Wi-Fi enabled computer. You can store these files for processing (see Figure 4-9 on page 36).

Four different file types containing 1-D XRD data can be created and downloaded, depending on the xrdDataType setting. The types are: .TXT, .MDI, .UXD, and .PLV. .TIF files can also be downloaded:

  • .TXT — Contains a generic form of the XRD data suitable for import into most available pattern matching software.
  • .MDI — Contains the XRD data specific for import into MDI Jade software.
  • .UXD — For import into Bruker software.
  • .PLV — For import into XPowder software.
  • .TIF — Contains the 2-D pattern image.


Table 10 on page 36 lists all of the available file types.



Settings Tab

In the Settings tab, you can edit the default data acquisition settings, or create custom modes of analysis. This allows you to modify the default data acquisition settings to create an analytical parameter set that is uniquely designed for the application at hand. For example, the signal-to-noise ratio improves with the summation of additional scans. Therefore, complex materials, or those with anticipated low concentrations of a given phase, would benefit by having a relatively high number of acquisitions scans.

To edit default settings

  1. In the Defaults area (see Figure 4-10 on page 38), click in a text box, and then change the value.
  2. Scroll through the list and change other values as desired. See Table 11 on page 38 for a complete list of default data acquisition settings.
  3. Scroll to the end of the list, then click Update Defaults.




To create a custom mode

  1. In the Custom Modes area, click Add New Mode (see Figure 4-10 on page 38).
  2. In the Add New Mode dialog box (see Figure 4-11 on page 40), click the Name text box, and then enter a name.
  3. Clear the default? check box preceding the data acquisition value text box you want to change.
  4. Click the text box, and then change the value.
  5. Scroll through the list, and then change other values as desired.
  6. Scroll to the end of the list, and then click Create Set.


To edit a custom mode

  1. In the Custom Modes area, select a custom mode, and then click edit (see Figure 4-10 on page 38).
  2. In the Editing Mode dialog box (see Figure 4-11 on page 40), clear the default? check box preceding the data acquisition value text box you want to change.
  3. Click in the text box, and then change the value.
  4. Scroll through the list, and then change other values as desired.
  5. Scroll to the end of the list, and then click Update Set.

To delete a custom mode

  1. In the Custom Modes area, select a custom mode, and then click delete (see Figure 4-10 on page 38).
  2. In the confirmation dialog box, click OK.

To upload firmware updates to the BTXII from your Wi-Fi enabled device.

  1. In the Upload Firmware area, click Browse, and then navigate to the update file computer (Figure 4-10 on page 38).
  2. Click Upload File.

XRD Analyzer Maintenance

Cleaning and Maintenance

This chapter describes the basic maintenance you must perform on the BTX II X-ray Diffraction Analyzer unit. The maintenance operations explained below enable you to keep your instrument in good physical and working condition. By virtue of its design, the BTX II X-ray Diffraction Analyzer only requires minimal maintenance. The chapter covers preventative maintenance and instrument cleaning.


The BTX II does not contain any user-serviceable parts. Do not disassemble or modify the system.

To clean the front panel

  • Clean the top of the BTX II with a soft, dry cloth.

Appendix A: Specifications

The BTX II X-ray Diffraction Analyzer operating characteristics differ depending on the operating temperature. The BTX II consumes more power at higher ambient temperature as it cools the CCD X-ray detector.

xrd-analyser-btx ii specifications

Appendix B: About Powder XRD Testing

The most commonly used crystallographic approach of XRD is powder X-ray diffraction (PXRD). The sample in PXRD is a powdered (polycrystalline) material, which is composed of many small crystallites that randomly assume all possible orientations with respect to the incident beam. In a PXRD experiment a relatively small proportion of the grains contribute to a given diffracted beam. Higher numbers of randomly oriented grains exposed to the X-ray lead to better statistical representation for any given diffraction direction. This is referred to as particle statistics.

Powder X-ray diffraction instruments require limited analytical volume to provide good resolution, so particle statistics are achieved using very fine grains of typically less than a few tens of micrometers. Particle statistics become even more critical with miniature systems because of the reduced size of their analytical volume. Conditions for good particle statistics vary, depending on parameters such as the symmetries in the crystal 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 statistics. This is achieved in the BTX II with sub-micron powders that lead to continuous Debye rings when using static samples. Very spotty rings are observed for grain sizes above 10 µm (the term spottiness is often used to refer to insufficient particle statistics).

When the grain size of the sample is not small enough to guarantee appropriate particle statistics, means to increase the number of crystal orientations effectively analyzed must be applied. This is typically done by translating or rotating the sample in the beam to analyze a larger amount of material or explore more orientations of the same grains. A novel method employed in the BTX II consists of placing the granular sample in motion using granular convection in vibrated cells. This method is very effective at improving particle statistics and allows analysis of materials with a grain size of up to 150 µm. This sample handling method relaxes the constraints on sample preparation by allowing grains nearly two orders of magnitude larger than ideal to be analyzed, while facilitating loading and removal of the powder.

See Figure B-1 on page 48. In example A, (a still sample) partial diffraction rings and Laue spots are observed. In example B, with granular convection, complete diffraction rings are observed (i.e. perfect powder pattern).


Appendix C: Data Analysis

Data analysis is accomplished using the XPowder application software. This software is supplied with your BTX II on the USB flash drive. This section includes instructions on installing the software and using it to verify alignment of the system using a quartz sample (also supplied). You can apply the same basic process of analyzing the quartz sample to analyze a wide range of other powdered substances.

To install XPowder

  1. Connect the USB flash drive (supplied) to a USB port of a computer.
  2. Find the xpowder_setup.exe filer, and then double-click the icon to run the program.
  3. Follow the instructions in the setup wizard (see Figure C-1 on page 49) as the installation progresses.


4. When the installation is complete, copy the registration code from the “License key” document on the USB flash drive.
5. Click Main menu > Help > XPowder registration code and paste the license key in the text box.

To load the DIFDATA 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 50).
  3. Under Click database file, select the Difdata.txt file.
  4. In the Database file extension list, click the down arrow, and then select .txt.
  5. Under Default scanning interval (Angstroms), in the Higher d-spacing box, type 70.00, and then, in the Lower d-spacing box, type 1.64.
  6. In the Database nickname box, type AMCSD.
  7. Select Add a new Database.
  8. Click 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 page 51.
  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 Wavelength setup dialog box (see Figure C-4 on page 51).
    The Wavelength setup dialog box is used to set the X-ray tube type, and automatically displays only on initial software setup.
  5. From the X-ray tube anode list, select either Co or Cu.
    The selection depends on the type of X-ray tube in your system.
  6. Click OK.

To analyze the test data

  1. In the XPowder menu, click Action > Background subtraction to display the Background subtraction dialog box (see Figure C-5 on page 52).
  2. Without changing any of the parameters, click Do it!
  3. Click Yes in the confirmation dialog box.
  4. On the XPowder tool bar, click Advanced searching.
    The advanced searching window containing a diffractogram 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 52).
    The purpose of decreasing or increasing the amount of background subtraction is to eliminate as much noise as possible while preserving as many peaks as possible.
  6. In the Searching parameters area, set the 2-theta gap to 0.30 (see Figure C-7 on page 53).
  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 superimposed (see Figure C-8 on page 54). The dialog box name is based on the name of the CCD image file exported from the BTX II. In Figure C-8, the dialog box name is RemoteTst-film in AMCSD.
  9. In the Least squares fitting area of the dialog box, click the Automatic check box. The XPowder 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.
    In many cases, this is another isomer of the same crystal/phase.
  11. Click Unchecks to eliminate unchecked (unwanted) phases (see Figure C-9 on page 54).
  12. Click Display card to inspect the phase details (see Figure C-10 on page 55).
  13. In the XPowder window, click Quantitative > LS-RIR Database Cards to view a relative intensity ratio semiquantitative analysis and summary (see Figure C-11 on page 55).
  14. To view a log report, click File > Save log file as TXT to generate a text file record of the session.

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