Introduction This guidance outlines procedures recommended by Bruker AXS for instrument verification. The procedures described apply to all Bruker AXS D8 ADVANCE, D8 DISCOVER, and D8 ENDEAVOR diffraction systems used for X-ray powder diffraction analysis in reflection mode and fully cover the functionality of all validation relevant components of these diffraction systems as provided in the following table.
(EQ) process as defined by GxP regulations. If your laboratory is not required to comply with GxP regulations you may skip this section. For instrument qualification Bruker AXS recommends the adaptation of the specifications and procedures provided in this booklet into your in-house EQ system according to the following schema: Table 1.2: Instrument performance verification as part of equipment qualification...
An instrument passing all tests with respect to line position, intensity and shape is automati- cally fit for all kinds of X-ray analysis. For GxP regulated laboratories Bruker AXS recommends to use the procedures provided in this chapter as a base for the creation of in-house SOPs.
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Procedures Table 2.1: Instrument parameters for Bragg-Brentano systems (incl. TWIN / TRIO Bragg-Brentano setting) Instrument Parameter Value Value (with air scatter screen) 3) 5) 3) 5) Generator settings Cu: 40 kV / 40 mA Cu: 40 kV / 40 mA 3) 5) 3) 5) Co: 35 kV / 40 mA Co: 35 kV / 40 mA Divergence slit 0.3°...
Procedures 2.4.2 Instruments Without Focusing Monochromator For instruments without primary beam monochromator the impact of the K component of the α2 radiation emitted by the X-ray source has to be taken into account. In order to achieve line in- tensities as accurate as possible, the complete K doublet must be used.
NIST SRM1976c origin to fit to a large variety of sample stages, as it is very stable, robust, long lasting, and does not require any preparation. The certificate is dedicated to Cu-radia- tion. However, Bruker AXS uses the d-spacing of this standard also for verifying angular ac- curacy (line-position and FWHM) for Co-radiation.
Reference Values Table 3.1: Reference values for line positions and relative intensities for Cu-radiation (CuK α1 λ = 0.154059 nm) Reflection Line position 2θ [°] Line position 2θ [°] Relative intensity (Net area rounded Bragg-Brentano Parallel Beam to 2 decimal place) 0 1 2 25.575 25.561 23.88...
Reference Values 3. The deflection angle must be saved to data base of the MEASUREMENT SUITE by the Save configuration to data base of the Configuration plugin. ´ The software will ask for a name for this configuration. The name is Instrument Verification Factory.
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Reference Values Table 3.4: Maximum allowed values for the line shape in terms of FWHM (Co-radiation). SC: scintillation counter, SOL‑XE: energy dispersive solid state detector, position sensitive detector VÅNTEC‑1, SSD160, LYNXEYE / LYNXEYE XE / LYNXEYE XE‑T, LYNXEYE-2, SSD160-2 and EIGER2 R 500K Reflection Bragg-Brentano Parallel Beam (Göbel Mirror) SC / SOL‑XE VÅNTEC‑1...
(for installations outside North America) D8 DISCOVER User Manual Vol. 2 DOC-M88-EXX162 D8 DISCOVER Supplement Folder DOC-M88-EXX163 D8 Series IQ OQ PQ for D8 ADVANCE / D8 DISCOVER DOC-M88-EXX160 D8 ENDEAVOR IQ OQ PQ DOC-M88-EXX265 LYNXEYE and SSD160 User Manual DOC-M88-EXX095 LYNXEYE XE User Manual...
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References – Glossary – Appendices A to I Glossary Certified reference material A reference material, accompanied by a certificate, one or more of whose property values are certified by a procedure, which establishes its traceability to an accurate realization of the unit in which the property values are expressed, and for which each certified value is accompanied by an uncertainty at a stated level of confidence.
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in Bragg-Brentano reflection geometry. The factory acceptance test proce- dure consists in full-profile measurements of the certified NIST standard reference material SRM1976c.
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A. Factory Acceptance Test Protocol Comments 22 / 96 DOC-M88-EXX157_V17_04.2019...
A. Factory Acceptance Test Protocol Part I: Instrument Details (D8 Series) Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractome- D8 ADVANCE Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes)
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A. Factory Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector (SOL‑XE) SOL‑XE User Manual DOC-M88-EXX113 VÅNTEC‑1...
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A. Factory Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractometer D8 DISCOVER Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) TXS Power: 50 kV / 100 mA (for 0.3x3 mm filament, line and spot focus) TXS Power: 50 kV / 22 mA (for 0.1x1 mm filament, spot focus) Vertical...
Part II: Angular Accuracy, Instrument Response and Resolution (D8 Series) Anode: Cu Bragg-Brentano Geometry Angular Accuracy: Difference Reference Position corr Instrument Response: I Instrument Resolution Maximum allowed 2θ deviation depends on height Maximum allowed intensity deviation for point detectors ± 10% FWHM <...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in Bragg-Brentano reflection geometry. The factory acceptance test proce- dure consists in full-profile measurements of the certified NIST standard reference material SRM1976c.
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B. Factory Acceptance Test Protocol Comments 32 / 96 DOC-M88-EXX157_V17_04.2019...
B. Factory Acceptance Test Protocol Part I: Instrument Details (D8 Series) Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes)
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B. Factory Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector SOL‑XE User Manual DOC-M88-EXX113 (SOL‑XE)
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B. Factory Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractometer D8 DISCOVER Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer Theta/2Theta Height: Radius: Primary radius ....[mm] Secondary radius ....[mm] Horizontal...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in parallel beam reflection geometry (Göbel mirror systems). The factory ac- ceptance test procedure consists in full-profile measurements of the certified NIST standard reference material NIST SRM1976c .
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C. Factory Acceptance Test Protocol Comments 42 / 96 DOC-M88-EXX157_V17_04.2019...
C. Factory Acceptance Test Protocol Part I: Instrument Details Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer...
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C. Factory Acceptance Test Protocol Instrument Details Set Values for Validation VÅNTEC‑1 VÅNTEC‑1 User Manual DOC-M88-EXX072 EIGER2 R 500K EIGER2 R 500K User Manual DOC-M88-EXX293 including D8 ADVANCE ECO 40 kV / 25 mA in case of D8 ADVANCE ECO Comments 44 / 96 DOC-M88-EXX157_V17_04.2019...
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C. Factory Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractome- D8 DISCOVER Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) TXS Power: 50 kV / 100 mA (for 0.3x3 mm filament, line and spot focus) TXS Power: 50 kV / 22 mA (for 0.1x1 mm filament, spot focus) Vertical...
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C. Factory Acceptance Test Protocol Instrument Details Set Values for Validation Slits Primary axial Soller slit 2.5° Secondary equatorial Soller slit 0.2° Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2...
Part II: Angular Accuracy, Instrument Response and Resolution Anode: Cu Parallel Beam Geometry Angular Accuracy: Difference Deflection angle corr Instrument Response: I Instrument Resolution Maximum allowed 2θ deviation depends on height Maximum allowed intensity deviation for point detectors ± 10% FWHM <...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in parallel beam reflection geometry (Göbel mirror systems). The factory ac- ceptance test procedure consists in full-profile measurements of the certified NIST standard reference material NIST SRM1976c .
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D. Factory Acceptance Test Protocol Comments 50 / 96 DOC-M88-EXX157_V17_04.2019...
D. Factory Acceptance Test Protocol Part I: Instrument Details Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer...
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D. Factory Acceptance Test Protocol Instrument Details Set Values for Validation VÅNTEC‑1 VÅNTEC‑1 User Manual DOC-M88-EXX072 EIGER2 R 500K EIGER2 R 500K User Manual DOC-M88-EXX293 1) including D8 ADVANCE ECO 2) 35 kV / 28 mA in case of D8 ADVANCE ECO Comments 52 / 96 DOC-M88-EXX157_V17_04.2019...
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D. Factory Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractome- D8 DISCOVER Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer Theta/2Theta Height: Radius: Primary radius ....[mm] Secondary radius ....
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D. Factory Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector (SOL‑XE) SOL‑XE User Manual DOC-M88-EXX113 VÅNTEC‑1...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in Bragg-Brentano reflection geometry. The factory acceptance test proce- dure consists in full-profile measurements of the certified NIST standard reference material SRM1976c.
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E. Customer Acceptance Test Protocol Comments 58 / 96 DOC-M88-EXX157_V17_04.2019...
E. Customer Acceptance Test Protocol Part I: Instrument Details (D8 Series) Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractome- D8 ADVANCE Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes)
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E. Customer Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector (SOL‑XE) SOL‑XE User Manual DOC-M88-EXX113 VÅNTEC‑1...
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E. Customer Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractometer D8 DISCOVER Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) TXS Power: 50 kV / 100 mA (for 0.3x3 mm filament, line and spot focus) TXS Power: 50 kV / 22 mA (for 0.1x1 mm filament, spot focus) Vertical...
Part II: Angular Accuracy, Instrument Response and Resolution (D8 Series) Anode: Cu Bragg-Brentano Geometry Angular Accuracy: Difference Reference Position corr Instrument Response: I Instrument Resolution Maximum allowed 2θ deviation depends on height Maximum allowed intensity deviation for point detectors ± 10% FWHM <...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in Bragg-Brentano reflection geometry. The factory acceptance test proce- dure consists in full-profile measurements of the certified NIST standard reference material SRM1976c.
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F. Customer Acceptance Test Protocol Comments 68 / 96 DOC-M88-EXX157_V17_04.2019...
F. Customer Acceptance Test Protocol Part I: Instrument Details (D8 Series) Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes)
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F. Customer Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector SOL‑XE User Manual DOC-M88-EXX113 (SOL‑XE)
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F. Customer Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractometer D8 DISCOVER Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer Theta/2Theta Height: Radius: Primary radius ....[mm] Secondary radius ....[mm] Horizontal...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in parallel beam reflection geometry (Göbel mirror systems). The factory ac- ceptance test procedure consists in full-profile measurements of the certified NIST standard reference material NIST SRM1976c .
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G. Customer Acceptance Test Protocol Comments 78 / 96 DOC-M88-EXX157_V17_04.2019...
G. Customer Acceptance Test Protocol Part I: Instrument Details Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer...
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G. Customer Acceptance Test Protocol Instrument Details Set Values for Validation EIGER2 R 500K EIGER2 R 500K User Manual DOC-M88-EXX293 including D8 ADVANCE ECO 40 kV / 25 mA in case of D8 ADVANCE ECO Comments 80 / 96 DOC-M88-EXX157_V17_04.2019...
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G. Customer Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractome- D8 DISCOVER Tube Power: 40 kV / 40 mA (for FL tubes) Tube Power: 40 kV / 30 mA (for FF tubes) TXS Power: 50 kV / 100 mA (for 0.3x3 mm filament, line and spot focus) TXS Power: 50 kV / 22 mA (for 0.1x1 mm filament, spot focus) Vertical...
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G. Customer Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter (See User LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 Manuals) LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector (SOL‑XE) SOL‑XE User Manual DOC-M88-EXX113 VÅNTEC‑1...
Part II: Angular Accuracy, Instrument Response and Resolution Anode: Cu Parallel Beam Geometry Angular Accuracy: Difference Deflection angle corr Instrument Response: I Instrument Resolution Maximum allowed 2θ deviation depends on height Maximum allowed intensity deviation for point detectors ± 10% FWHM <...
Serial Number: SAP Number (Sales Order Number): This protocol details the results of the factory acceptance test procedure for Bruker AXS dif- fraction systems in parallel beam reflection geometry (Göbel mirror systems). The factory ac- ceptance test procedure consists in full-profile measurements of the certified NIST standard reference material NIST SRM1976c .
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H. Customer Acceptance Test Protocol Comments 86 / 96 DOC-M88-EXX157_V17_04.2019...
H. Customer Acceptance Test Protocol Part I: Instrument Details Instrument Configuration D8 ADVANCE Instrument Details Set Values for Validation Diffractometer D8 ADVANCE Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer...
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H. Customer Acceptance Test Protocol Instrument Details Set Values for Validation VÅNTEC‑1 VÅNTEC‑1 User Manual DOC-M88-EXX072 EIGER2 R 500K EIGER2 R 500K User Manual DOC-M88-EXX293 1) including D8 ADVANCE ECO 2) 35 kV / 28 mA in case of D8 ADVANCE ECO Comments 88 / 96 DOC-M88-EXX157_V17_04.2019...
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H. Customer Acceptance Test Protocol Instrument Configuration D8 DISCOVER Instrument Details Set Values for Validation Diffractome- D8 DISCOVER Tube Power: 35 kV / 40 mA (for FL tubes) Tube Power: 35 kV / 30 mA (for FF tubes) Vertical Theta/Theta goniometer Theta/2Theta Height: Radius: Primary radius ....[mm] Secondary radius ....
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H. Customer Acceptance Test Protocol Instrument Details Set Values for Validation Detector Scintillation counter LYNXEYE, SSD160 LYNXEYE User Manual DOC-M88-EXX095 LYNXEYE XE LYNXEYE XE User Manual DOC-M88-EXX240 LYNXEYE XE‑T LYNXEYE XE‑T User ManualDOC-M88-EXX239 LYNXEYE‑2 LYNXEYE‑2 User Manual DOC-M88-EXX305 SSD160-2 SSD160-2 User Manual DOC-M88-EXX306 Solid state detector (SOL‑XE) SOL‑XE User Manual DOC-M88-EXX113 VÅNTEC‑1...
I. Daily Check Protocol I. Daily Check Protocol System No.: Sample: Anode: Reflection (hkl): 2θ : Maximum allowed FWHM : Maximum allowed 2θ deviation: ± 0.01° FWHM (< FWHM Date Line Line Intensity Line Shape Pass / Fail Operator Signature Postion DOC-M88-EXX157_V17_04.2019 93 / 96...
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I. Daily Check Protocol Date Line Line Intensity Line Shape Pass / Fail Operator Signature Postion 94 / 96 DOC-M88-EXX157_V17_04.2019...
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