A software platform for XRD analysis in industrial, pharmaceutical or GLP/GMP environments

X’Pert Industry software

The Analytical X-ray Company

Optimizing your manufacturing processes

X’Pert Industry

X’Pert Industry is a software package for routine quantitative and qualitative analysis by X-ray diffraction (XRD) in an industrial environment.

XRD is an invaluable tool for supporting all kinds of production processes. Historically, XRD had limited use for production purposes because of the long data collection and analysis times required. Nowadays, high-speed detectors like PANalytical’s X’Celerator, combined with sophisticated software algorithms have reduced sample turnaround time to a few minutes only.

A few examples of industrial use of XRD are: • Phasecompositionofclinkersandcementinthebuilding

materials industry• Controloftheelectrolyticbathsinaluminiumproduction• Analysisofrespirablesilica• Percentagecrystallinitydeterminationinpharmaceuticals• andmanymore

Depending on the application, the analysis is fully done in X’Pert Industry, or automatically coupled to advanced analysis programs such as X’Pert HighScore Plus. The analysis can be set up in such a way, that operators without expert knowledge can do the analysis.

X’Pert Industry is the product of years of listening and responding to the needs of our process control customers.

PANalytical understands the needs of its process control customers:

• Push-buttoncontrolforoperators• Fullycustomizable• Differentlanguageversioncapability

combined with security levels• Exampleanalysisprogramsincludedfor

common applications, such as aluminium bath and respirable silica analysis

• Unattendedscheduledoperations,suchas monitor and check sample measurement

• Supportsmethoddevelopmenton X’Pert PRO MPD instruments with

multiple optical configurations• Statisticalprocesscontrolcharting

capability• SupportsFDA21CFRPart11• EnhancedsecurityforGLP/GMP• OptionalAuditTrailsoftware• Asymmetricscancapabilityfor

quantitative analysis of films • Supportsmultipleopticalconfigurations

on an X’Pert PRO MPD system

Schedule regularly occurring actions to happen unattended

Visual display of sample changers and samples with names allows you to quickly assess progress of your batch of samples for XRD analysis.

Automation ready

Easytouse

XRDML – the way forward in XRD data storage

The XRDML file format is based on XML technology, with a published protocol (www.XRDML.com). XRDML files contain the complete measurement description, including X-ray optical components and their parameters, allowing complete experiment traceability. XML can be opened in any text editor software. This gives your data long term viability.

X’Pert Industry can be controlled from a remote site using an automation network. Remote control and reporting can be arranged via the Universal Automation Interface (UAI) included on the X’Pert Industry installation CD. This allows complete automation setup, from the combination of XRD with sample preparation equipment to other analytical instruments, such as X-ray fluorescence (XRF) spectrometers.

X’Pert Industry is designed for ease-of-use by anyone. The custom tool bar allows push-button operation. Method development is made easy by a command wizard that helps you write programs and add logic loops for intelligence. A global variable table enables occasional refreshing of, for example, a blank filter sample measurement needed in a routine analysis calculation.

X’Pert Industry – the choice for a wide range of current and previous generation PANalytical products

Create your own custom toolbar for push-button start of routine operations

Pharmaceutical process control

aPPLICatIon foCus

PANalytical uses the company’s many years ofexperienceworkinginenvironmentsabidingbythisFDAregulationtobringyousolutions for regulated XRD process control.

These include:• Irrevocable21CFRPart11securitymode

in X’Pert Industry• AuditTrailsoftware• IQ/OQproductswithcertifiedstandards• Worldwideapplicationsupportand

expertise

XRPD is an important analysis tool for the development, scale-up and production of pharmaceutical materials, providing information on: polymorphic phases and excipient phases present, impurities, sample crystallinity, and crystallite size. X’Pert Industry can automate these processes, for quantitative analysis of phase composition or qualitative analysis for polymorphs present in a sample. Reports can be generated and transmitted to LIMS systems automatically.

Automatic identification of phases present in a sample, and reporting to LIMS or anywhere on your network made possible by X’Pert Industry in conjunction with X’Pert HighScore (Plus) software

Pharmaceutical process controlX’Pert Industry supports the X’Pert PRO MPD XRD system, with multiple optical configuration capability. This system can be configured with parallel beam optics for quantitative analysis on a curved surface such as a tablet.

X’Pert Industry can also perform grazing incidence scans for analysis of thin films and coatings.

Calibration curve from XRD data collected from curved tablets with parallel beam geometry

Secureoperationinamulti-userenvironment

Maintaining system and data security in a multi-user environment is made easy through X’Pert Industry’s customizable security settings and user administration. Audit trailing software and IQ/OQ validation packages are available, together with worldwide application support knowledgeable in compliant operation. X’Pert Industry is also at the heart of the CubiX Walk-Up, the first multi-user walk up XRD system for secure environments.

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1.1

1.2

1.3

11 12 13 14 15 16

Indomethacin Conc. [%]

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R2 = 0.9897

User administration with access levels and preferred language interface

Customizable security levels

Cement production control

aPPLICatIon eXPertIse

XRD is becoming the preferred method for fast and accurate analysis of clinker and cement phase concentrations. X’Pert Industry offers seamless integration of full phase analysis by the Rietveld method, free lime analysis by calibration method, automatic reporting and trend ticker display, as well as the ability to include XRD in full robotic automation schemes. Additionally, XRD can be a valuable tool for monitoring the quality and variability of raw feed, limestone, alternative fuels, slag and fly ash.

Benefits of XRD• Improvedquality/

process control • Measurablecostsavings: - Eliminationoffree

lime titration - Improved kiln control - Good clinker

characterization, more predictable properties

- Analysis of cement grinding, blending and dispatch processes

- Monitoring of limestone addition

Quantitative analysis of cement by Rietveld

Twinned operation of PANalytical’s CubiX FAST XRD and Axios Cement XRF

Position [°2Theta] (Copper (Cu))20 30 40 50 60

Co

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0

5000

10000Alite 61.3 %Belite 12.1 %Ferrite 10.9 %Free Lime 0.0 %Alum_cub 2.9 %Alum_ortho. 0.5 %Periclase 0.6 %Arcanite 1.7 %Portlandite 0.8 %Calcite 6.8 %Quartz 0.0 %Gypsum 1.3 %Hemihydrate 1.1 %Anhydrite 0.0 %

0

10000

20000

30000Co

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Position [°2Theta]36.50 37 37.50 38

7.5%CaO

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C3S0 5 10 15 20 25 30 35 40 45 50

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y = -7.042 x +0.21x - 0.702, =r 0.9985

Free lime calibration from standards

Catalyst production

aPPLICatIon eXPertIse

X’Pert Industry controls catalyst production by monitoring unit cell size, percent crystallinity and phases present in production samples. The Import/Export feature allows plants to share methods easily. Statistical Process Control (SPC) charts can monitor the catalyst production process over any length of time.

XRD is the standard method for automated analysis of the ratio of phases in the production of aluminium metal, with measurement times of one minute for a typical sample. X’Pert Industry includes features specifically for the aluminium industry, such as a cell age tracker and a corrections table for automatic instructions for dosing of a pot to correct the bath ratio. X’Pert Industry can also make use of a calcium XRF channel option on PANalytical XRD systems to simultaneously monitor elemental Ca concentration while measuring phase concentrations by diffraction.

Portion of analysis program to determine unit cell size

Correction table and calibration curve for fluorite

SPC chart of unit cell size with 2 sigma, 3 sigma and mean displayed

Aluminium bath control

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Report results your way

X’Pert Industry offers extensive reporting options, including enhanced graphics capability, conditional texts, evaluations of expressions and remote destinations. Example reports can be customized with your company or lab logo, or a new report form can be built using a report generation wizard. The reporting destinations are independent of the site from where the program is controlled, and multiple destinations can be set up on a per sample or per batch basis.

Report generation tools, including a wizard and an SQL interface, are part of X’Pert Industry’s ultimate flexibility in report design.

PANalytical B.V.

Lelyweg 1, 7602 EA AlmeloP.O. Box 13, 7600 AA AlmeloThe NetherlandsT +31 (0) 546 534 444F +31 (0) 546 534 598 info@panalytical.comwww.panalytical.com

Regional sales offices

AmericasT +1 508 647 1100 F +1 508 647 1115Europe, Middle East, AfricaT +31 (0) 546 834 444 F +31 (0) 546 834 499Asia PacificT +65 6741 2868 F +65 6741 2166

Global and near

Quantitative Analysis and Resolution Test Page 1of 1

Date:28-Jan-2008 16:13 SR M 1976 -

The quantitative analysis test determines the relative intenisties of the reflectionsof NIST SRM 1976 . The deviation of the relative differences must be less than 8 % .

Angle Relative intensity Measured Exp.determined Difference Relative Differenceas given by NIST Intensity Relative intensity

deg. 2theta % cps * deg.2theta % % %

25.5 32.34 200.70 34.61 2.27 7.01

35.1 100.00 579.95 100.00 0.00 0.0043.3 51.06 315.48 54.40 3.34 6.5452.5 26.69 162.61 28.04 1.35 5.0557.5 92.13 537.65 92.71 0.58 0.63

76.8 & 77.2 55.57 306.51 52.85 -2.72 -4.8989.0 11.76 Not measured95.2 10.14 Not measured

Intensity distribution (relative difference): 7.01 OKRelative difference between -4.89 and 7.01

The resolution is determined at the reflection at 57.5 degree 2theta.The full width at half maximum (FWHM) must be less than or equal to 0.10 deg.

FWHM: 0.068Resolution: OK

57.2 57.4 57.6 57.8 58.00.

50000.

100000.

Angle (2Theta)

OQ-QRes-200703071546Counts

X'Pert Industry 2.0 OQ_Resolution_Test.RDE