BS en 15305-2008 Non-Destructive Testing - Test Method For Residual Stress Analysis by X-Ray Diffraction

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BRITISH STANDARD BS EN 15305:2008
Non-destructive
Testing — Test Method
for Residual Stress
Licensed Copy: :FULLNAME, : DATE, Uncontrolled Copy, (c) BSI
analysis by X-ray
Diffraction
ICS 19.100
NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

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BS EN 15305:2008
National foreword
This British Standard is the UK implementation of EN 15305:2008.

The UK participation in its preparation was entrusted to Technical
Committee WEE/46, Non-destructive testing.
A list of organizations represented on this committee can be obtained on
request to its secretary.
This publication does not purport to include all the necessary provisions
of a contract. Users are responsible for its correct application.
Compliance with a British Standard cannot confer immunity
from legal obligations.
This British Standard Amendments/corrigenda issued since publication

was published under
the authority of the
Standards Policy and Date Comments
Strategy Committee on 30
September 2008
© BSI 2008
ISBN 978 0 580 55634 0

BS EN 15305:2008
EUROPEAN STANDARD EN 15305

NORME EUROPÉENNE
EUROPÄISCHE NORM August 2008
ICS 19.100
English Version
Non-destructive Testing - Test Method for Residual Stress

analysis by X-ray Diffraction
Essais non-destructifs - Méthode d'essai pour l'analyse des Zerstörungsfreie Prüfung - Röntgendiffraktometrisches
contraintes résiduelles par diffraction des rayons X Prüfverfahren zur Ermittlung der Eigenspannungen
This European Standard was approved by CEN on 4 July 2008.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15305:2008: E
worldwide for CEN national Members.
BS EN 15305:2008
EN 15305:2008 (E)
Contents Page
Foreword..............................................................................................................................................................5
Introduction .........................................................................................................................................................6
1 Scope ......................................................................................................................................................7
2 Normative references ............................................................................................................................7
3 Terms, definitions and symbols...........................................................................................................8
3.1 Terms and definitions ...........................................................................................................................8
3.2 Symbols and abbreviations ..................................................................................................................8
4 Principles..............................................................................................................................................10
4.1 General principles of the measurement ............................................................................................10
4.2 Biaxial stress analysis ........................................................................................................................12
4.3 Triaxial stress analysis .......................................................................................................................13
5 Specimen ..............................................................................................................................................14
5.1 Material characteristics .......................................................................................................................14
5.1.1 General..................................................................................................................................................14
5.1.2 Shape, dimensions and weight ..........................................................................................................15
5.1.3 Specimen composition/homogeneity ................................................................................................15
5.1.4 Grain size and diffracting domains....................................................................................................16
5.1.5 Specimen X-ray transparency ............................................................................................................16
5.1.6 Coatings and thin layers .....................................................................................................................16
5.2 Preparation of specimen.....................................................................................................................17
5.2.1 Surface preparation .............................................................................................................................17
5.2.2 Stress depth profiling..........................................................................................................................17
5.2.3 Large specimen or complex geometry..............................................................................................17
6 Equipment ............................................................................................................................................17
6.1 General..................................................................................................................................................17
6.2 Choice of equipment ...........................................................................................................................18
6.2.1 General..................................................................................................................................................18
6.2.2 The ω-method .......................................................................................................................................19
6.2.3 The χ-method .......................................................................................................................................20
6.2.4 The modified χ-method .......................................................................................................................21
6.2.5 Other geometries .................................................................................................................................21
6.3 Choice of radiation ..............................................................................................................................21
6.4 Choice of the detector .........................................................................................................................23
6.5 Performance of the equipment...........................................................................................................24
6.5.1 Alignment .............................................................................................................................................24
6.5.2 Performance of the goniometer .........................................................................................................24
6.6 Qualification and verification of the equipment ...............................................................................24
6.6.1 General..................................................................................................................................................24
6.6.2 Qualification .........................................................................................................................................24
6.6.3 Verification of the performance of the qualified equipment ...........................................................26
7 Experimental Method ..........................................................................................................................27
7.1 General..................................................................................................................................................27
7.2 Specimen positioning .........................................................................................................................27
7.3 Diffraction conditions..........................................................................................................................28
7.4 Data collection .....................................................................................................................................29
8 Treatment of the data ..........................................................................................................................30
8.1 General..................................................................................................................................................30
8.2 Treatment of the diffraction data........................................................................................................30
8.2.1 General..................................................................................................................................................30
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8.2.2 Intensity corrections ...........................................................................................................................30

8.2.3 Determination of the diffraction line position...................................................................................31
8.2.4 Correction on the diffraction line position........................................................................................32
8.3 Stress calculation................................................................................................................................32
8.3.1 Calculation of strains and stresses...................................................................................................32
8.3.2 Errors and uncertainties [16], [17] .....................................................................................................33
8.4 Critical assessment of the results .....................................................................................................34
8.4.1 General .................................................................................................................................................34
8.4.2 Visual inspection .................................................................................................................................34
8.4.3 Quantitative inspection.......................................................................................................................34
9 Report ...................................................................................................................................................35
10 Experimental determination of XECs ................................................................................................36
10.1 Introduction..........................................................................................................................................36
10.2 Loading device ....................................................................................................................................37
10.3 Specimen..............................................................................................................................................37
10.4 Loading device calibration and specimen accommodation ...........................................................38
10.5 Diffractometer measurements ...........................................................................................................38
10.6 Calculation of XECs ............................................................................................................................38
11 Reference specimens..........................................................................................................................39
11.1 Introduction..........................................................................................................................................39
11.2 Stress-free reference specimen.........................................................................................................39
11.2.1 General .................................................................................................................................................39
11.2.2 Preparation of the stress-free specimen...........................................................................................39
11.2.3 Method of measurement .....................................................................................................................40
11.3 Stress-reference specimen ................................................................................................................40
11.3.1 Laboratory qualified (LQ) stress-reference specimen.....................................................................40
ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
11.3.2 Inter-laboratory qualified (ILQ) stress-reference specimen............................................................41
12 Limiting cases......................................................................................................................................41
12.1 Introduction..........................................................................................................................................41
12.2 Presence of a subsurface stress gradient ........................................................................................42
12.3 Surface stress gradient.......................................................................................................................42
12.4 Surface roughness ..............................................................................................................................42
12.5 Non-flat surfaces .................................................................................................................................42
12.6 Effects of specimen microstructure ..................................................................................................43
12.6.1 Textured materials...............................................................................................................................43
12.6.2 Multiphase materials ...........................................................................................................................43
12.7 Broad diffraction lines ........................................................................................................................44
Annex A (informative) Schematic representation of the European XRPD Standardisation Project ........46
Annex B (informative) Sources of Residual Stress .......................................................................................47
B.1 General .................................................................................................................................................47
B.2 Mechanical processes ........................................................................................................................47
B.3 Thermal processes..............................................................................................................................47
B.4 Chemical processes............................................................................................................................47
Annex C (normative) Determination of the stress state - General Procedure............................................48
C.1 General .................................................................................................................................................48
C.2 Using the exact definition of the deformation ..................................................................................49
C.2.1 General .................................................................................................................................................49
C.2.2 Determination of the stress tensor components .............................................................................49
C.2.3 Determination of θ and d0 ...................................................................................................................50
C.3 Using an approximation of the definition of the deformation.........................................................50
C.3.1 General .................................................................................................................................................50
C.3.2 Determination of the stress tensor components .............................................................................51
C.3.3 Determination of θ0 and d0 ..................................................................................................................51
Annex D (informative) Recent developments.................................................................................................52
D.1 Stress measurement using two-dimensional diffraction data........................................................52
D.2 Depth resolved evaluation of near surface residual stress - The Scattering Vector Method......54
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D.3 Accuracy improvement through the use of equilibrium conditions for determination of
stress profile ........................................................................................................................................55
Annex E (informative) Details of treatment of the measured data ...............................................................56
E.1 Intensity correction on the scan ........................................................................................................56
E.1.1 General..................................................................................................................................................56
E.1.2 Divergence slit conversion .................................................................................................................56
E.1.3 Absorption correction .........................................................................................................................57
E.1.4 Background correction .......................................................................................................................58
E.1.5 Lorentz-polarisation correction..........................................................................................................58
E.1.6 K-Alpha2 stripping...............................................................................................................................59

E.2 Diffraction line position determination..............................................................................................59
E.2.1 Centre of Gravity methods..................................................................................................................59
E.2.2 Parabola Fit ..........................................................................................................................................60
E.2.3 Profile Function Fit ..............................................................................................................................60
E.2.4 Middle of width at x% height method ................................................................................................61
E.2.5 Cross-correlation method...................................................................................................................61
E.3 Correction on the diffraction line position ........................................................................................61
E.3.1 General..................................................................................................................................................61
E.3.2 Remaining misalignments ..................................................................................................................61
E.3.3 Transparency correction.....................................................................................................................62
Annex F (informative) General description of acquisition methods ............................................................64
F.1 Introduction ..........................................................................................................................................64
F.2 Definitions ............................................................................................................................................64
F.3 Description of the various acquisition methods ..............................................................................67
F.3.1 General method....................................................................................................................................67
F.3.2 Omega (ω ω) method...............................................................................................................................68
F.3.3 Chi (χχ) method......................................................................................................................................69
F.3.4 Combined tilt method (also called scattering vector method)........................................................71
F.3.5 Modified chi method ............................................................................................................................73
F.3.6 Low incidence method ........................................................................................................................76
F.3.7 Modified omega method .....................................................................................................................77
F.3.8 Use of a 2D (area) detector .................................................................................................................78
F.4 Choice of Φ and Ψ angles ...................................................................................................................79
F.5 The stereographic projection .............................................................................................................80
Annex G (informative) Normal Stress Measurement Procedure" and "Dedicated Stress
Measurement Procedure.....................................................................................................................82
G.1 Introduction ..........................................................................................................................................82
G.2 General..................................................................................................................................................82
G.2.1 Introduction ..........................................................................................................................................82
G.2.2 Normal stress measurement procedure for a single specimen......................................................82
G.2.3 Dedicated Stress Measurement Procedure for very similar specimens........................................82
Bibliography ......................................................................................................................................................84
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EN 15305:2008 (E)
Foreword
This document (EN 15305:2008) has been prepared by Technical Committee CEN/TC 138 “Non-destructive
testing”, the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by February 2009, and conflicting national standards shall be withdrawn
at the latest by February 2009.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This European Standard about “Non destructive testing - X-ray diffraction from polycrystalline and amorphous
material” is composed of:
 EN 13925-1, General principles;
 EN 13925-2, Procedures;
 EN 13925-3, Instruments;
 EN 1330-11, Non-destructive testing - Terminology - Terms used in X-ray diffraction from polycrystalline
and amorphous materials
In order to explain the relationship between the topics described in the different standards, a diagram
illustrating typical operation involved in XRPD is given in Annex A.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
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EN 15305:2008 (E)
Introduction
Residual strains in crystalline materials may be determined by X-ray diffraction analysis. Assuming linear
elastic distortions, the related residual stresses are calculated.
In this document the principles of the measure procedure and the analysis technique are described.
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EN 15305:2008 (E)
1 Scope
This European Standard describes the test method for the determination of macroscopic residual or applied
stresses non-destructively by X-ray diffraction analysis in the near-surface region of a polycrystalline
specimen or component.
All materials with a sufficient degree of crystallinity can be analysed, but limitations may arise in the following
cases (brief indications are given in Clause 12):
 Stress gradients;
 Lattice constants gradient ;
 Surface roughness;
 Non-flat surfaces (see 5.1.2);
 Highly textured materials;
 Coarse grained material (see 5.1.4);
 Multiphase materials;
 Overlapping diffraction lines;
 Broad diffraction lines.
The specific procedures developed for the determination of residual stresses in the cases listed above are not
included in this document.
The method described is based on the angular dispersive technique with reflection geometry as defined by EN
13925-1.
The recommendations in this document are meant for stress analysis where only the diffraction line shift is
determined.
This European Standard does not cover methods for residual stress analyses based on synchrotron X-ray
radiation and it does not exhaustively consider all possible areas of application.
Radiation Protection. Exposure of any part of the human body to X-rays can be injurious to health. It is
therefore essential that whenever X-ray equipment is used, adequate precautions should be taken to protect
the operator and any other person in the vicinity. Recommended practice for radiation protection as well as
limits for the levels of X-radiation exposure are those established by national legislation in each country. If
there are no official regulations or recommendations in a country, the latest recommendations of the
International Commission on Radiological Protection should be applied.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
EN 13925-1:2003, Non-destructive testing – X-ray diffraction from polycrystalline and amorphous material –
Part 1: General principles
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EN 15305:2008 (E)
EN 13925-2:2003, Non-destructive testing – X-ray diffraction from polycrystalline and amorphous materials –
Part 2: Procedures.
EN 13925-3:2005, Non-destructive testing – X-ray diffraction from polycrystalline and amorphous materials –
Part 3: Instruments
ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results – Part 1: General
principles and definitions
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
3 Terms, definitions and symbols

For the purposes of this document, the following term, definition and symbols apply
3.1 Terms and definitions
3.1.1
Residual stress
self-equilibrating internal stresses existing in a free body which has no external forces or constraints acting on
its boundary
3.2 Symbols and abbreviations

2θ
θ
beams. ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
The diffraction angle; this is the angle between the incident and diffracted X-ray
The Bragg angle; this is the angle between the diffracting lattice planes and the
incident beam.
 ω The angle between the incident X-ray beam and the specimen surface at χ = 0.
 φ The angle between a fixed direction in the plane of the specimen and the projection
in that plane of the normal to the diffracting lattice planes.
 ψ The angle between the normal of the specimen and the normal of the diffracting
lattice planes.
 χ The angle χ rotates in the plane perpendicular to that containing ω and 2θ; the
rotation axis of χ is orientated perpendicular to both the ω and the ϕ axis.
 {hkl Family of crystal lattice planes defined by the indices h, k and l.
 εφψ Strain measured in the direction defined by the angles φ and ψ.
 d0 Interplanar distance (d spacing) of a strain free specimen.
 dφψ Interplanar distance (d spacing) of strained material in the direction of measurement

defined by the angles φ and ψ.
 (S1, S2, S3) Specimen coordinate system.
 (L1, L2, L3) Laboratory coordinate system.
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EN 15305:2008 (E)
1
 2 S2{hkl}, S1{hkl} Elasticity constants of the family of lattice planes {hkl.
 σii Normal stress components (i = 1,2,3).
 τij Shear stress components (i ≠ j ; i,j = 1,2,3).
 Z Distance to the surface of the specimen.

 z X-ray penetration depth.
 LP The Lorentz Polarization factor.
 A The Absorption factor.
 ILQ Inter-Laboratory Qualified (used in connection with stress-reference specimen).
 LQ Laboratory Qualified (used in connection with stress-reference specimen).
 σcert Certified normal stress value of the ILQ stress-reference specimen.
 τcert Certified shear stress value of the ILQ stress-reference specimen.
 σref Normal stress value of the LQ specimen.
 τref Shear stress real value for the LQ specimen.

Lref
σdetermined
Average width of the diffraction lines for the LQ specimen.
Determined Normal stress value of the stress-reference specimen.
 τdetermined Shear stress value determined for the stress-reference specimen.
 Ldetermined The average width of the diffraction line determined for the stress-reference
specimen.
 u( ) Standard uncertainty in the normal stress.
 u(τ) Standard uncertainty in the shear stress.
 rσcert, rτ cert, Repeatability of the normal stress, shear stress, and line width respectively of the
certified ILQ stress- rLcert reference specimen.
 rσref, rτref , Repeatability of the normal stress, shear stress, and line width respectively of the LQ
stress-reference rLref specimen.
 Rσcert, Rτcert Reproducibility of the normal stress and shear stress.
 λ Wavelength of the X-rays used.
 Tr(σ) Trace of the stress tensor: Tr(σ) = Σσii.
 I hkl Net integrated intensity of the hkl diffraction line.
 XECs X-ray elasticity constants.
 sr and sR Standard deviations of the repeatability and reproducibility.
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EN 15305:2008 (E)
 β Integral breadth.
 σφ Normal stress value in a direction defined by the angle φ.
 τφ Shear stress value in a direction defined by the angle φ.
NOTE Elasticity constant is also referred to as elastic constants.

4 Principles
4.1 General principles of the measurement
Key
S1, S2 axes in the plane of the specimen; S1 is defined by the operator

S3 axis normal to the specimen surface
L1, L2, L3 laboratory coordinate system; L3 is normal to the diffracting lattice planes {hkl} and it is the
bisector of the angle between incident and diffracted beams
φ angle between a fixed direction in the plane of the specimen and the projection in that plane of
the normal to the diffracting lattice planes
ψ angle between the normal of the specimen and the normal of the diffracting lattice planes
Sφ direction in which the stresses σφ and τφ are measured
Figure 1 — Orthogonal coordinate systems relevant to XRD stress determination
On the basis of elasticity theory, for a macroscopically isotropic crystalline material the formula to express the
strain in the direction defined by the angles φ and ψ (see Figure1) is:
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BS EN 15305:2008
EN 15305:2008 (E)
= S1{hkl }[σ 11 + σ 22 + σ 33 ] + S2{hkl }σ 33 cos 2 ψ + S2{hkl }[σ 11 cos2 φ + σ 22 sin 2 φ + τ 12 sin 2φ ]sin 2 ψ +
{hkl } 1 1
ε φψ
2 2
1 {hkl }
+ S2 [τ 13 cos φ + τ 23 sin φ ]sin 2ψ
2
(1a)
Τhe stress components σφ and τφ are defined respectively as the normal stress and the shear stress in the Sφ
direction (see Figure 1):
σ φ = [σ 11 cos 2 φ + σ 22 sin 2 φ + τ 12 sin 2φ ] (1b)
τ φ = [τ 13 cos φ + τ 23 sin φ ] (1c)
where the symbols of the formulae (1a), (1b), and (1c) are
εφψ{hkl} strain in the direction defined by the angles φ and ψ for the family of lattice planes
{hkl};
1 {hkl }
S1{hkl } and S2 X-ray elasticity constants for the family of lattice planes {hkl};
2
σ11, σ22, σ33 normal stress components in the directions S1, S2 and S3 (cf. Figure 1);
τ12 shear stress within the plane defined by S1 and S2;
τ13
τ23
φ
shear stress within the plane defined by S1 and S3;
shear stress within the plane defined by S2 and S3;
angle between a fixed direction in the plane of the specimen and the projection in
that plane of the normal to the diffracting lattice planes;
ψ angle between the normal of the specimen and the normal of the diffracting lattice
planes;
σφ normal stress component in a direction defined by the angle φ;
σ11, σ22 normal stress components in the directions S1, S2;
τφ shear stress value in a direction defined by the angle φ.
The strain εφψ may be expressed in terms of lattice spacings according to the formula:
{hkl } d   sin θ 0 
ε φψ = ln φψ  = ln  (2a)
 sin θ 
 d0   φψ 
or alternatively by the approximate formulae:
{hkl }  d φψ − d 0 
ε φψ ≅   (2b)

 d0 
or
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BS EN 15305:2008 中国工业检验检测网 http://www.industryinspection.com
EN 15305:2008 (E)
ε φψ {hkl } ≅ −cot (θ 0 )∆θφψ (2c)
where
dφψ spacing of the family of lattice planes {hkl} with their normal in the direction defined by φ and ψ;
d0 strain-free lattice spacing of the same family of lattice planes {hkl};
θ0 Bragg angle associated to d0;

θφψ Bragg angle associated to dφψ.
The formula (2c) is approximate and therefore it should not be used. In the calculation using (2b) the value d0
2
can be estimated by interpolation on the fitted d vs. sin ψ curve (for details see Annex C). Using formula (2a)
the d 0 and θ0 values do not need to be accurately known.
Since the penetration depth of X-rays in most materials is in the order of tens of micrometers, σ33=0 can often
be assumed. Care should be exercised in the case of large penetration depths or multiphase materials (see
Clause 12).
Thus, equation (1) can be simplified:
ε φψ {hkl } = S1{hkl }[σ 11 + σ 22 ] + S 2{hkl }[σ 11 cos 2 φ + σ 22 sin 2 φ + τ 12 sin 2φ ]sin 2 ψ +

1
2
(3)
1 {hkl }
+ S 2 [τ 13 cos φ + τ 23 sin φ ]sin 2ψ
2
where the symbols are as for formulae (1a), (1b), (1c). ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
For the usual methods (ω and χ method, see Clause 6.2) the rotation angle φ is equal to the rotation applied to
the specimen around the surface normal. Other methods exist in which the relations between the angles φ, ψ
and the specimen rotations are more complex (see Annex F).
Note that the elasticity constants of the {hkl} lattice planes may be significantly different from those of the
macroscopic bulk values (see Clause 10).
4.2 Biaxial stress analysis
From X-ray diffraction experiments on polycrystalline materials εψφ values at different ψ and φ angles are
obtained. If the stress state is biaxial (τ13 = τ23 = σ33 = 0), then it follows from equation (3) that the dependence
of εφψ on sin ψ is linear:
2
1 {hkl}
ε φψ{hkl} = S2 .σφ sin ψ + S1{hkl}.Tr(σ)
2
(4a)
2
where:
Tr(σ) =(σ11+σ22).
For formula (4a) the same symbols hold as for formula (3).
If the stress state is biaxial then experimentally a straight line should be obtained (see Figure 2).
The stress in the φ -direction, σφ, is calculated from the slope of the straight line:
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中国工业检验检测网 http://www.industryinspection.com BS EN 15305:2008
EN 15305:2008 (E)
 ∂ε φψ {hkl } 
 
 ∂sin 2 ψ 
 
σφ = {hkl } (4b)
1
2
S2
Key
εφψ strain measured in the direction defined by the angles φ and ψ
ψ
angle between the normal of the specimen surface and the normal of the diffracting lattice planes
2
Figure 2 — Example of εψφ versus sin ψ plot at constant φ in case of biaxial stress.
In Figure 2 the material undergoes a stress state with σφ = -400 MPa, τφ = 0. The X-ray elasticity constant of
the material is:
1 -6 -1
S2{hkl}= 6.8 10 MPa (4c)
2
The σφ values for negative and positive ψ values are coinciding and denoted by squares. The line corresponds
to the least square fitting by equation (4a).
Due to the insufficient accuracy of d0, the stresses obtained from Τρ(σ) should not be used for further
calculations.
4.3 Triaxial stress analysis
If shear stresses acting in the planes perpendicular to the specimen surface are present (τ13 ≠ 0 and/or τ23 ≠
2
0) then the plot of ε φψ vs. sin ψ is an ellipse, showing the “ψ-splitting” for ψ>0 and ψ<0 (see Figure 3). If σ33 is
2
not equal to zero then the slope of sin ψ plot is proportional to σφ −σ33. In these cases, equation (4a) becomes:
1 {hkl} 1 1 {hkl}
S2{hkl}.τφ sin2ψ + ⋅S2 .σ33 + S1{hkl}. Tr(σ)
2
ε φψ = S2 (σφ −σ33)sin ψ + (5)
2 2 2
where
Tr(σ) =(σ11+σ22 +σ33)
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BS EN 15305:2008
EN 15305:2008 (E)
Key
εφψ
ψ ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
strain measured in the direction defined by the angles φ and ψ
angle between the normal of the specimen surface and the normal of the diffracting lattice
planes
+ positive ψ values
▲ negative ψ values
2
ψφ versus sin ψ plot at constant φ in case of triaxial stress (ψ
Figure 3 — Example of εψ ψ splitting).
In Figure 3 the material undergoes a stress state with σφ = - 400 MPa, τφ = - 50 MPa. The X-ray elasticity
-6 -1
constant of the material is ½ S2{hkl} = 6.8 x 10 MPa . The lines correspond to the least square fitting by
equation (5).
At a fixed φ angle, the σφ and τφ values are obtained by the least squares fitting of the strain data with equation
(5). By measuring at least three different φ directions and at least three ψ angles the stress tensor can be
derived (see Clause 7.4).
5 Specimen
5.1 Material characteristics
5.1.1 General
To measure and calculate the residual stress the following parameters are required:
 crystallographic data of the material;
 X-ray elasticity constants of the material.
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When the values of the X-ray elasticity constants have not been determined experimentally (see Clause 10), it
is recommended to use X-ray elasticity constants calculated by models taking into account single crystal
elastic anisotropy and the coupling conditions between the crystallites (see Clause 8.3.1.2). Incorrect values
of the X-ray elasticity constants (½ S2{hkl} and S1{hkl}) may cause significant systematic errors in the stresses
calculated.
Prior knowledge of the specimen history and its microstructure can indicate if problems might occur as listed
in Clause 1 (see Clause 12).
5.1.2 Shape, dimensions and weight

For any specimen, a suitable flat region should be chosen for residual stress measurement. The shape and
size of the specimen is not critical, but it shall fit onto the specimen stage when required.
The specimen is subjected to various tilts during the measurement and therefore needs to be firmly attached
to the specimen stage. Care has to be taken on maximum allowable weight for the goniometer and on how the
specimen is to be mounted and held onto the goniometer. The specimen can be clamped to the stage only if
this does not lead to additional stresses being induced into the specimen.
The necessary flatness of the specimen depends on the irradiated area. It is recommended that the local
radius of curvature of the specimen shall be large enough (see Clause 12) to allow for an irradiation as longer
as possible.
5.1.3 Specimen composition/homogeneity
Care shall be taken to choose an irradiated volume with homogeneous composition when possible. Since the
penetration depth of the X-rays as well as irradiated area depend on ψ tilt, consideration shall be given to
compositional changes that may be present within the surface and the depth (see Clause 6.3).
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In multiphase materials the residual stress, i.e. the overall residual stress, is determined from the contributions
of the stresses present in all specific phases using:
σ overall = ∑xσ
phases
i i (6)
where
overall
σ is the residual stress of the specimen;
xi is the volume fraction of the i phase;
σi is the stress in the i phase obtained from the {hkl} lattice planes of that phase.
It is therefore mandatory that the phases are known from which the diffraction lines originate.
5.1.4 Grain size and diffracting domains
The grain size in the irradiated volume can also affect the residual stress value. In many crystalline materials
grain sizes are in the range 10-100µm. As grains often consist of many diffracting domains, such grain size
values are usually acceptable for X-ray stress measurements. For larger grain sizes, it is likely that only a few
diffracting domains contribute to the diffraction line. This can lead to large variations in the peak shape and
intensity with φ, ψ directions. In addition, the presence of micro/intergranular strains may also affect the results.
In some cases it is possible to reduce this effect by oscillating the specimen (for details see Clause 7),
because this increases the number of diffracting grains.
5.1.5 Specimen X-ray transparency
In some materials the penetration depth of X-rays can be large enough to lead to errors in stress
measurements due to the offset of the irradiated volume with respect to the surface (see Annex E). In addition,
the effect of stress gradients and significant stress σ33 will be more pronounced.
5.1.6 Coatings and thin layers
Residual stresses in coatings can be determined provided that the diffraction lines associated with the coating
itself can be identified and isolated from the diffraction lines associated with the substrate.
Measurement in thin layers may lead to the following problems:
 low diffracted intensities and/or insufficient grain statistics;
 additional diffraction phenomena from multilayers;
 overlap with a diffraction line from the substrate;
 steep stress gradient;
 strong texture.
(See also Clause 12.)
Finally, the values of the elasticity constants for the coating may be significantly different from the ‘bulk’ values.
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5.2 Preparation of specimen
5.2.1 Surface preparation
Surface preparation should be avoided. However, if the surface is oxidized, painted or varnished, it can be
cleaned by electro polishing or by using chemicals to preserve the stress field as much as possible. Be careful
with chemicals which may weaken the grain boundaries or which may preferentially etch one of the phases
present as it can lead to local stress relaxation.
5.2.2 Stress depth profiling
5.2.2.1 General
The stress can be determined as a function of depth by successive cycles of electro polishing and stress
analysis. In some cases also a variation of the penetration depth of the X-ray, e.g. by using different
wavelengths or by tilting of the specimen, can furnish depth profile stress data.
5.2.2.2 Removal of surface layers
Any mechanical or electro discharge machining (EDM) method to remove surface layers induces residual
stresses, altering the stress field of the surface. Thus, such methods shall be avoided. Chemical attack or
electro polishing is suggested to remove layers without introducing new stresses on the surface. Both
chemical attack and electro polishing may cause relaxation of the residual stresses, e.g. due to the removal of
stress in the surface layer, changes of surface roughness, or grain boundary attack. When necessary, thick
layers can be removed using a combined machining or grinding procedure, followed by electro polishing to
remove the layer strained by the machining or grinding. If the volume of the removed material is large
compared to the total volume of the specimen, stress redistribution effects shall be considered in the
5.2.2.3 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
calculation of the original stress field. Simple cases are treated in [2].
Evaluation of the thickness reached after removal of the material
The thickness of the layer removed shall be determined. It is suggested that the shape and the roughness of
the surface are verified because problems may arise from non-flat and/or rough surface (see Clause 12).
5.2.3 Large specimen or complex geometry
Generally it is recommended to avoid the sectioning of samples. If sectioning of the sample is necessary then
this should be carried out with care to avoid changes in the existing residual stresses. The measured region
shall, if possible, be far enough from the edge of the specimen to avoid any effect of relaxation of residual
stress perpendicular to the edge. It is recommended that the distance to the edge is at least equal to the
thickness of the specimen.
In addition, one should avoid overall relaxations which may occur, e.g., when cutting pipes in the axial
direction. If relaxations are expected, methods such as strain gauging [3] should be used to monitor any
changes during or after cutting.
6 Equipment
6.1 General
A general description of the equipment used for residual stress analysis can be found in EN 13925-3. In this
chapter some specific aspects of the equipment that relate to the analysis of residual stresses are discussed.
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6.2 Choice of equipment
6.2.1 General
In the general case two rotations are required (see Figure 1); ψ rotation is strictly necessary while φ-rotation
can be useful in some experiments. The general arrangement of a laboratory goniometer measuring at high
2θ angles, as used in residual stress analysis, is shown in Figure 4.
Key
S1, S2, S3 specimen coordinate system
θ Bragg angle, this is the angle between the diffracting lattice planes and the incident beam
2θ diffraction angle, this is the angle between the incident and diffracted X-ray beams
ωR rotation about the ω axis
φR rotation about the φ axis
χR rotation about the χ axis
SP specimen
D detector
X X-ray tube
Figure 4 — Goniometer at Ψ = 0 for χ and ω method (ω

ω = θ, χ=0)
The ψ tilt can be performed in various geometries. Two of them, called ω and χ method, are shown in Figures
5 and 6.
Laboratory goniometers achieve a good precision in the measurement, permitting generally an extensive
choice of 2θ angles; they are often used in other applications of X-ray diffraction (texture, profile analysis,
phase analysis, (see EN 13925-1)). However, generally only non-cumbersome specimens can be analysed.
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6.2.2 The ω-method
In this method (also called iso-inclination method) the specimen is rotated (tilted) about the ω axis. Both ω and
2θ are in the same plane. To obtain ω values, ψ values are algebraically added to θ. Absolute values of ψ are
added to θ for positive ψ or subtracted for negative ψ. Most conventional powder diffractometers, with a de-
coupled ω drive (where ω and 2θ axes are able to move independently) can make measurements using this
method. The geometry is shown schematically in Figure 5.
Note that the σφ direction lies in the plane of diffraction (see also Annex E).
Key
θ Bragg angle; this is the angle between the diffracting lattice planes and the incident beam
2θ diffraction angle, this is the angle between the incident and diffracted X-ray beams
ωR rotation about the ω axis
φR rotation about the φ axis
X X-ray tube
SP Specimen
D detector
Figure 5 — The ω-method: ψ angle is achieved through ω rotation where φ = 0 and Ψ = ω - θ = - 45° (χ
χ
remains equal to zero)
Positive and Negative Offsets
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Figure 6a shows a specimen with a positive ψ-offset for the ω-method, where ψ has been added to θ. Figure
6b shows a negative ψ-offset where ψ has been subtracted from θ.
Key
2θ diffraction angle; this is the angle between the incident and diffracted X-ray beams
θ Bragg angle; this is the angle between the diffracting lattice planes and the incident beam
ω angle between the incident X-ray beam and the specimen surface at χ = 0
φ angle between a fixed direction in the plane of the specimen and the projection in that plane of the normal
to the diffracting lattice planes
A diffracting lattice planes
B
C
D
sample at
incident x-ray beam
diffracted x-ray beam
Figure 6a — Positive ψ-offset (ω
ω = θ + ψ, with ψ>0) Figure 6b — Negative ψ-offset (ω
ω = θ + ψ, with ψ<0)
When the ω-method is used with the negative ψ-offset, the decreased incidence angle increases the
“defocusing” effects which increase the broadening of the diffraction lines and decrease the intensities more
than an equal but positive ψ at the same 2θ. However, both positive and negative ψ-offsets shall be used
when shear stresses shall be evaluated. In this case measurements at negative ψ tilts can be avoided by
rotating the specimen (around the φ axis) by 180° and then measure the stress using positive ψ tilts. This
avoids problems caused by defocusing and/or the higher sensitivity to alignment errors with negative ψ tilts.
From the point of view of stress analysis, it is equivalent to negative ψ measurements without a φ rotation
(often referred to as pseudo-negative tilting).
For focusing optics, measurements applying negative ψ are more susceptible to misalignments than
measurements applying positive ψ.
6.2.3 The χ-method
Note that the σφ direction is perpendicular to the plane of diffraction (see also Annex E).
Mechanically the χ-method is more complex and, for some diffractometers, it requires the incorporation of
additional equipment (such as an Eulerian cradle). Negative ψ can also be reached by rotation about φ axis of
180° and applying positive ψ.
The advantage in using the χ-method is that defocusing effects are the same for positive and negative ψ.
Generally the χ-method leads to smaller errors related to the specimen centring than for the ω−method.
This method is sometimes confusingly referred to as the ψ method.
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6.2.4 The modified χ-method
The modified χ-method is mainly applied in portable diffractometers in conjunction with two position sensitive
detectors. The specimen is rotated about the χ axis, which is in a plane normal to that containing ω and 2θ. At
χ = 0 the incident beam is normal to the surface of the specimen which corresponds to ω = 90°. Two detectors
are used and these are placed symmetrically with regard to the incident beam.
In the case of the one-detector system using the χ geometry for the χ = 0 position the normal on the diffracting
lattice planes and on the sample are parallel, whereas in the case of the two-detector system the incident
beam is parallel to the normal on the diffracting lattice planes.
The ψ angle is achieved through χ rotation but ω remains equal to 90° instead of θ, i.e. at χ = 0, the incident
beam is normal to the surface of the specimen. Thus, cos ψ = cosχsinθ. Starting position (left) and position for
χ = 50°(right), the measurement is performed for φ = 90°(the strains obtained from the two detectors shall be
averaged and the appropriate corrections shall be performed).
Key ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
L3 normal to the diffracting {hkl} lattice planes
2θ diffraction angle; this is the angle between the incident and diffracted X-ray beams
χ angle χ rotates in the plane perpendicular to that containing ω and 2θ; the rotation axis of χ is
orientated perpendicular to both the ω and the ϕ axes
Figure 7 — The modified χ-method
6.2.5 Other geometries
The geometries presented in Figures 5 and 6 are the more common geometries. Other geometries are
possible, but not considered in detail in this document. A general approach describing some geometries is
given in Annex F.
6.3 Choice of radiation
The choice of X-ray tube anode and therefore the wavelength of the incident X-ray beam is critical for the
determination of residual stress.
If the Kα1 radiation in the incident beam causes fluorescence from the specimen, the wavelength is not
suitable, because the fluorescence produces a very high background and consequently poor peak-to-
background ratio. This can be dramatically improved by using e.g. a diffracted beam monochromator, which
removes the fluorescent radiation before the detector, or by using an electronic energy discriminating detector.
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Moreover, when the incident X-ray beam is absorbed by fluorescence effects, the penetration depth into the
specimen can be very small and insufficient for a stress value representative of the specimen.
Usually, in this case, a longer wavelength can be chosen, which does not have sufficient energy to cause
fluorescence.
The average information depth is defined as:

sin 2 θ − sin 2 (ω − θ )
z= for ω-method
2µ sin θ cos(ω − θ )
(7a)
sinθ cos χ
z= for χ-method (7b)
2µ
z=
(
cos χ 1 − cot 2 θ ) for modified χ-method
2µ
(7c)
where for formulae (7a), (7b), (7c)
z is the X-ray penetration depth;

θ is the Bragg angle;
ω is the angle between the incident X-ray beam and the specimen surface at χ = 0;
χ
µ ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ
is the angle χ rotates in the plane perpendicular to that containing ω and 2θ;
is the linear attenuation coefficient.
For other geometries, adequate formulae shall be used (see Annex F).
Examples of diffraction conditions (e.g. radiation to be used, filter, {hkl} lattice planes, Bragg angle) for
common materials are reported in Table 1.
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Table 1 — Diffraction conditions for common materials
a
Alloy Crystal Anode Kβ filter {hkl} 2θ(°) Multiplicity Average
structure of the information
lattice depth of X-rays
planes in µm at:
ab
ψ=0
Nickel alloys cubic Mn Cr {311} 152 to 162 24 4.9
Ferritic steels cubic Cr V {211} 156 24 5.8
Cast iron (matrix)

Austenitic steels cubic Mn Cr {311} 152 24 7.2
Aluminium alloys cubic Cr V {311} 140 24 11.5
Aluminium alloys cubic Cu Ni {422} 137 24 35.5
Cobalt alloys cubic Mn Cr {311} 153 to 159 24 5.6
Copper alloys cubic Mn Cr {311} 149 24 4.2
Titanium alloys hexagonal Cu Ni {213} 142 24 5.0
Molybdenum cubic Fe Mn {310} 153 24 1.6
alloys
Zirconium alloys hexagonal Fe Mn {213} 147 24 2.8
Tungsten alloys cubic Co Fe {222} 156 8 1.0
Alumina - alpha rhomboed Cu Ni {146} 136 12 37.4
ric {4.0.10} 145 6 38.5
Fe Mn {2.1.10} 152 12 20.0
Alumina - gamma cubic Cu Ni {844} 146 24 38.5
V Ti {440} 128 12 8.8
a
Indicative values.
b
Average information depth is defined as the depth from which 67% of the diffracted intensity has been absorbed. It is
the depth at which the stress is evaluated if the stress gradient along the depth is linear.
The X-radiation should be selected to give a reflection at a Bragg angle greater than 130° 2θ. However,
though not ideal, it is possible to use reflections which are as low as 120° 2θ. Using reflections with 2θ angles
of less that 120° is not recommended because of the low sensitivity of strain measurement and in the case of
focusing optics also the high sensitivity to misalignment.
The diffraction line should not be too close to the high 2θ limit of the instrument: if possible, the whole
diffraction line down to the background at both sides of the peak shall be recorded.
Depending on the set up of the diffractometer and the treatment of data, large errors can arise if these
conditions are not fulfilled [4].
Residual stresses calculated by using different wavelengths may have different values because of the
different penetration depth of the X-ray beam into the specimen. This is more an issue where steep stress
gradients are present (see Clause 12).
6.4 Choice of the detector
Detectors are different in type, size and shape (see 4.3 of EN 13925-3:2005)
The choice of spot, linear or area detector is important to reduce the measurement time and it may influence
some aspects of the setting geometry.
Spatial resolution of a linear or area detector is generally not an issue in stress analysis.
A good energy resolution helps to reduce the background and thus to obtain good line position repeatability.
Saturation of the detector shall be avoided because it distorts the shape of the diffraction lines.
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6.5 Performance of the equipment
6.5.1 Alignment
Primarily, the alignment shall be in accordance with the requirements of EN 13925-3. (Clause 7.1)
Additional requirements are:
 The surface of the specimen shall coincide with the axis of rotation of the specimen which depends on
whether the ω or χ method is used. For the ω-method the surface of the specimen shall coincide with the
ω-axis of the goniometer. For the χ-method it shall coincide with the χ-axis of the cradle.
 If several stress components are measured, the φ axis shall be coincident with the centre of the irradiated
area.
The incident X-ray beam shall intersect the axes of rotations φ and ψ. Displacement of the beam will introduce
positional errors during rotation and/or translation of the specimen. For the χ-method the displacement in the
axial direction is most important to minimize and for the ω-method it is the displacement in the equatorial
plane.
The alignment of the beam can be checked for example using a fluorescent screen, narrow aperture (glass
slit) or small reference specimen. The alignment shall be verified before performing the measurement. If the
perfect alignment of specimen height and beam is not achieved, the diffraction line positions can be corrected
afterwards by using data coming from either a reference specimen (see Clause 6.6 and E.3.1) or a thin layer
of fine well crystallised powder deposited on the surface of the specimen itself. A shift of the ψ origin cannot
be corrected by this procedure.
The weight of the specimen can affect the alignment of the system. Therefore the alignment shall be checked
by using a similar loading condition of the specimen stage.
6.5.2 Performance of the goniometer
Additionally to the demands presented in this document, the performance of the goniometer shall follow the
requirements of EN 13925-3. (Clause 5).
6.6 Qualification and verification of the equipment
6.6.1 General
The qualification and verification of the equipment is performed in accordance with EN 13925-3 (Clause 8):
 It is necessary to qualify new equipment or existing equipment after mechanical changes have been
made or if any changes to the electronics have occurred. Qualification is performed by measuring stress-
free and ILQ stress-reference specimens (see Clause 11.3).
 It is necessary to periodically verify the performance of the equipment. This verification is performed with
the stress-free and ILQ or LQ stress-reference specimens (see Clause 11.3).
An ILQ stress-reference specimen may be obtained through round robin tests of at least five laboratories in
accordance with ISO 5725-2. If certified specimens are available they should be used as ILQ stress-reference
specimen [5].
6.6.2 Qualification
6.6.2.1 General
The qualification shall be performed using both a stress-free specimen and an ILQ stress-reference specimen.
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6.6.2.2 Criteria of qualification of a stress free specimen
The measurement of a stress free specimen (see 11.2) allows the evaluation of the errors related to the
displacement of the beam and of the specimen.
Powder materials are expected to have zero stress: i.e. 2θ constant for all ψ and φ angles. If stress values
significantly different from zero are obtained, the system shall be checked, adjusted and then requalified.
The equipment is certified if the stress free specimen gives the following result:
1 1 1 1
σ ≤ ⋅ {hkl} with u (σ ) ≤ ⋅ (8a)
10000 1 2 S 2 10000 1 2 S 2{hkl}
1 1 1 1
τ ≤ ⋅ {hkl} with u (τ ) ≤ ⋅ (8b)
20000 1 2 S 2 20000 1 2 S 2{hkl}
where
1 {hkl}
S2 is the elasticity constants of the family of lattice planes{hkl};
2
u(σ) and u(τ) are the uncertainties as calculated in 8.3.2.
The value of 1 2S 2{hkl} used should be that of the analysed material, not that of the powder of the stress-free
specimen.
6.6.2.3
Qualification of an instrument with an ILQ stress-reference specimen
When available, the qualification shall be performed on an ILQ stress-reference specimen (see Clause 11.3).
If the obtained values are significantly different from the reference value, the equipment shall be checked,
adjusted and then requalified.
The qualification with an ILQ stress-reference specimen shall be performed in the following steps:
 Choose the number n (n > 4) of measurement to be done on the specimen in repeatable conditions (see
Clause 11.3.1.3) for the qualification (or the verification). The number n shall be reported.
 Calculation of the critical difference, CD, for the normal stress and for the shear stress:
1  n −1 1  n −1
CD σ = R σ 2 − rσ 2   and CD τ = R τ 2 − rτ 2   (9)
2  n  2  n 
 Realisation of n measurements σi and τi (i = 1 to n) on the ILQ specimen and calculation of the average
values:
1 n 1 n
σ= ∑σ i
n i =1
and τ= ∑τ i
n i =1
(10)
 The goniometer is considered qualified or verified if the two following conditions on the normal stress and
the shear stress are fulfilled:
σ ref −σ ≤CDσ and τ ref −τ ≤CDτ (11)
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where for formulae (9), (10), (11)
CD σ is the normal stress Critical Difference;
CD τ is the shear stress Critical Difference;
Rσ, Rτ are reproducibility values;
rσ, rτ are repeatability values (see also Clause 11.3.2);

σ is the average normal stress on n measurements;
σi is the normal stress of the i measurements;
τ is the average shear stress on n measurements;
τi is the average shear stress of the i measurements;

σref is the normal stress value of the LQ specimen;
τref is the shear stress real value for the LQ specimen.
6.6.3 Verification of the performance of the qualified equipment
6.6.3.1 General
The verification shall be performed using both a stress-free specimen and a stress-reference specimen (ILQ
or LQ).
6.6.3.2 Verification of the performance of an instrument with a stress free specimen
Verification with a stress free specimen.
Proceed as in 6.6.2.2
NOTE The choice of n can be different for a qualification and verification.
6.6.3.3 Verification of the performance of an instrument with a stress-reference specimen
If a LQ stress-reference specimen is used, the following criteria shall be verified:
 determined stress should satisfy:
rσ
σ ref − σ determined ≤ (12)
2
 determined shear stress should satisfy:
rτ
τ ref − τ determined ≤ (13)
2
 determined width of the line should satisfy:
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Lref − Ldetermined ≤ rL (14)

2
where for the formulae (12), (13), (14)
σref is the normal stress value of the LQ specimen;
σdetermined is the determined Normal stress value of the stress-reference specimen;

τref is the shear stress real value for the LQ specimen;
τdetermined is the shear stress value determined for the stress-reference specimen;
Lref is the average width of the diffraction lines for the LQ specimen;
Ldetermined is the average width of the diffraction line determined for the stress-reference specimen;
rσ, rτ, rL are the repeatabilities obtained by the laboratory on the internal specimen (see Clause 11.3.1.3).
If an ILQ stress-reference specimen is used, proceed as in 6.6.2.3.
7 Experimental Method
7.1 General
The following steps shall be followed when performing X-ray residual stress measurements:

Verification of the alignment of the diffractometer (see Clause 6.6) and, where appropriate, the calibration
of the detector;
 Positioning of the specimen (see Clause 7.2);
 Choice of diffraction conditions (see Clause 7.3);
 Choice of measurement conditions and data collection (see Clause 7.4);
 Visual check of the diffraction lines (see Clause 8.4.2);
 Data treatment (see Clause 8);
 Reporting (see Clause 9).
7.2 Specimen positioning
The angles between the specimen coordinates and the incident and diffracted X-ray beams define the residual
stress measurement direction.
The specimen to be measured shall be placed at the centre of rotation of the goniometer (see Clause 6.5.1);
the specimen should be oriented so that the stress being measured is in the direction of interest (see Figure 1).
When possible choose the irradiated surface area of the specimen to have a curvature as small as possible
and a negligible stress gradient in the plane of the surface (see Clause 12). The position of the irradiated area
should be defined precisely. The area can be kept constant by masking a part of the specimen e.g. using wax.
However, at high ψ angles, the thickness of the mask may induce a “shadow zone”, thus the ψ angle range
should be limited.
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The centre of the investigated area should be in the centre of rotation of the goniometer (see Clause 6.5.1)
within 10-100µm depending on the setup of the goniometer. An incorrect positioning with respect to the ψ
origin will lead to an inaccurate shear stress. The position of the specimen surface should be invariant to any
angular movement in φ or ψ. The positioning procedure can be checked with the help of reference specimens
during a verification operation as described in Clause 6.6.
7.3 Diffraction conditions

The phase considered and the indexing of the diffraction line to be used shall be known.
The diffracting lattice planes, the wavelengths and the instrumental conditions shall be chosen in order to
have:
 high diffraction angle;
 no overlapping diffraction lines;
 good background definition;
 adequate average information depth.
Commonly used conditions are given in Table 1 (Clause 6.3)
Microstructural effects (grain size, texture, multiphase material, etc.) or stress gradients can make it difficult or
even impossible to analyse the diffraction line. In these cases, stress values obtained by measurements made
on different phases or different crystallographic lattice planes may be different (see Clause 12).
In textured specimens often measurements on reflections with a high multiplicity are beneficial. If the
specimen has a large grain size it may also help to select a reflection with a high multiplicity and/or a
wavelength with a deeper penetration depth.
The prior knowledge of these problems helps with the choice of the best operating conditions to better
facilitate the treatment of the data.
For accurate comparisons with previous data/measurements it is useful to check the lattice planes and the
wavelengths previously used and, if possible, select the same ones.
For details see Clause 12.
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7.4 Data collection
The main parameters for data collection are:
a) Counting time and step size:
The counting time required to obtain a sufficiently accurate diffraction pattern (see Clause 8.4.2) will vary
depending on the tube, the optics, the detector (see EN 13925-3:2005 Clause 4.3), and specimen
characteristics.
Sufficient data points should be collected to describe the upper part of the line. The step size should be
between FWHM/20 and FWHM/10.
The choice of the measurement range and the background shall be in accordance with EN 13925-2:2003,
6.3.Care should be taken if another diffraction line is close to the measured peak. The diffraction range
should be limited so that the background subtraction is not perturbed. Sometimes not subtracting the
background gives better results than subtracting a poor estimation of the background.
b) Choice of φ and ψ angles:
If there is no shear stress τφ, i.e. in the plane normal to the specimen surface in the investigated φ
2
direction, at least four to five measurements in a range of sin ψ values to a value as large as possible
2
(typically 0.5 or more) and constant sin ψ steps are recommended. Due to defocusing problems or beam
overflow there is a practical limit to the maximum ψ value. For example in focusing geometry it is usually
taken 15° less than the theoretical limit (ψ= 90° for the χ -method and ψ = θ for the ω-method).
If a shear stress normal to the specimen surface in the investigated φ direction seems to be present, at
2
least 7 measurements in the sin ψ range are necessary with negative and positive values of ψ in order to
analyse the ψ-splitting. More than 9 measurements are recommended.
For the ω-method, pseudo-negative angles (i.e. positive ψ with additional 180° φ rotation) are
recommended when negative ψ tilts are required for the analysis of ψ-splitting. In this case, true negative
ψ angles (i.e. 'glancing'/small incident angle; large deflected angle) should be avoided because of the
strong sensitivity to specimen displacement and equatorial beam misalignment (even when these errors
are small).
If the principal directions are not known, full stress/tensor determination requires at least three
independent φ directions. The usual way to choose these directions is 0°, 45° and 90°. However it is
advisable to use a larger φ range and/or more independent φ angles. To obtain the uncertainties for the
stress values at least four φ values are required. The difference between the φ angles should be chosen
according to:
∆φ =180°/n
where
∆φ is the difference between the φ angles;
n is the number of independent φ angles.
2
For each φ at least 7 ψ directions in the ∆sin ψ range are necessary with negative and positive values of
ψ.
In contrast to the determination of stresses in particular directions φ, determination of the full stress tensor
requires the knowledge of the unstressed lattice spacing value, d0, with at least the precision needed to
calculate the stress normal to the specimen surface ( ∆ε about 1 part in 10 ).
5
c) Oscillations:
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This method can be applied to materials that have large domain sizes (such as castings, forged goods,
welds, etc.) with the aim of increasing the number of domains that contribute to the diffracted signal.
Generally the options are:
1) Oscillate the specimen around any axis (χ, ψ, φ, ω) to increase the number of grains meeting the
criterion for diffraction. The oscillations can be very large ± 10° or more [6]. However, oscillations
greater then 10° are not recommended. When specimen oscillations are used, the acquisition
time per step shall allow an integer number of complete oscillations.
For linear detectors, when used in the scanning mode, integration takes place over a range of ω-
angles which is equivalent to ω oscillation.
For area detectors, when the γ-integration is used to generate the diffraction profile, it actually
integrates the data collected in a range of various diffraction vectors (see Annex D) resulting in a
virtual oscillation.
2) Translate the specimen along S1 and/or S2 directions during the measurement in order to cover
a larger area of the surface. Translation during a measurement in both S1 and S2 directions can
give a marked improvement in the diffraction line profile.
NOTE When producing a stress map, this translation can not be used.
d) X-ray Tube Power:
The X-ray tube should in general be operating near its maximum recommended power output, so that the
diffraction line can be recorded in the minimum time possible.
8 Treatment of the data
8.1 General
The treatment of the data is described.
Analysis of the diffraction lines and calculation of the stress may be performed using proprietary software
supplied with the particular diffractometer being used or other software. It shall be verified that the software
used provides adequate tools for performing the data treatment as described in this Clause and for reporting
as described in Clause 9.
The complete treatment of the measurement data is subdivided into three stages:
1) Treatment of the diffraction data to obtain peak positions;
2) Stress calculation from peak positions;
3) Critical assessment of the results.
8.2 Treatment of the diffraction data
8.2.1 General
General treatments of diffraction data and analysis are reported in EN 13925-1:2003, Clause 6 and EN 13925-
2:2003, Clause 6, Annex D and Annex E.
8.2.2 Intensity corrections
A precise determination of the position of a diffraction line can be obtained after applying the appropriate
corrections to the intensities. The following corrections are commonly used:
 Divergence slit correction;
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 Absorption factor A;
 Lorentz-polarisation factor LP;
 Alpha2 stripping.
The details of diffraction data treatment are given in Annex E.
8.2.3 Determination of the diffraction line position

Several methods exist for the determination of the diffraction line position. The parameters of the chosen
method shall be specified. The most commonly used are:
a) Centre of Gravity method:
1) Classical Centre of Gravity;
2) Sliding Centre of Gravity;
3) Threshold Centre of Gravity;
4) Centred Centre of Gravity (Centred Centroid);
b) Polynomial fit:
1) 3-point parabola;
2) Multiple-point parabola;
3) Higher order polynomial;
c) Profile function fit:
1) Gauss;
2) Lorentz also called Cauchy;
3) Modified Lorentz (Pearson VII with m = 2);
4) Intermediate Lorentz (Pearson VII with m=1.5);
5) Pearson VII;
6) Pseudo-Voigt;
7) Voigt;
8) Pearson IV;
d) Middle of width at % height method:
1) Middle of FWHM (50% height);
2) Middle of 2/3 height (67% height);
e) Cross correlation method.
Other methods are also possible. The chosen method shall ensure good repeatability. Refer to Annex E for
details.
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8.2.4 Correction on the diffraction line position
In the case of a low absorbing material, transparency introduces a shift of the diffraction line position (see
Clause 5.1.5). The data shall be corrected (see Annex E.3.2).
When possible remaining not removable misalignment effects shall be calculated (EN13925-3:2005, Annex
C.2).
8.3 Stress calculation

8.3.1 Calculation of strains and stresses
8.3.1.1 Strain calculation
Formulae are given in 4.1.
8.3.1.2 Stress calculation
1) Choice of X-ray elasticity constants (XECs):
1 {hkl}
The XECs (S1{hkl} and S2 ) of the material under analysis should be experimentally obtained (see
2
Clause 10). They may also be calculated from mechanical models e.g. Kröner, Mori-Tanaka, Hill models
or taken from the literature. The use of the Voigt or Reuss models is not recommended.
The use of macroscopic elasticity constants is not recommended if the X-ray elasticity constants are
available.
1
S2{
hkl}
and S1{
hkl}
NOTE 1 Incorrect values of the X-ray elasticity constants ( ) used in the stress calculations can
2
cause significant systematic errors, because the calculated residual stress is proportional to the values of the X-ray
elasticity constants.
NOTE 2 X-ray elasticity constants should be experimentally determined (see Clause 10), because they may differ
by as much as 40% from the bulk values.
NOTE 3 The use of wrong XECs in the calculation of stress may be acceptable for comparative measurements.
The XEC’s used and their origin shall be reported.
2) Stress calculations:
a) Analysis in a single direction:
A straight line (equation (4a)) can be fitted to the data if no shear stress is present. Otherwise an ellipse
(equation (3)) shall be fitted.
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b) Tensor analysis:
An appropriate fitting procedure shall be used to fit equation (5).
8.3.2 Errors and uncertainties [16], [17]
8.3.2.1 General
Sources of errors and uncertainties can be:

 Material: microstructure, chemical homogeneity, stress homogeneity, etc.;
 Experimental parameters: diffraction parameters (see EN 13925-2), specific choices of φ, 2θ, χ and ω
angles, etc.;
 Assumptions of the chosen mechanical model: biaxial, triaxial, anisotropic model, etc.
In the report information shall be given on the method used to estimate uncertainty.
8.3.2.2 Errors
Errors should be kept as low as possible.
In addition to the issues mentioned in Clause 12 at least the following points shall be considered:
 beam misalignments,
 detector calibration (in the case of 1D or 2D position sensitive detectors),
 beam divergence,
 specimen displacement,
 procedures used for diffraction data treatment,
 mechanical models and methods used for stress calculation.
Some of these errors are smaller at high 2θ angles.
8.3.2.3 Uncertainties
The uncertainty is composed of several contributions. The most commonly considered contributions are:
 Counting statistics: the repeatability of the diffraction line position is mainly influenced by the height of the
peak, by the height to background ratio, and the height to noise ratio.
 Dispersion on strain values: it can be calculated from the standard deviation of the strain values by least
squares fitting.
Generally, standard deviations shall be given. A confidence interval can also be quoted.
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8.4 Critical assessment of the results
8.4.1 General
All the criteria listed in 8.4.2 and 8.4.3 shall be verified. If the criteria mentioned there are not fulfilled, one
shall:
1) verify not to be in a limiting case (see Clause 12);

2) reprocess the data (see Clause 8);
3) perform a new measurement.
8.4.2 Visual inspection
8.4.2.1 For a single diffraction line
Check for overlaps with neighbouring diffraction lines, truncations, irregular shape of the diffraction line and
the background.
8.4.2.2 For the complete set of diffraction measurements
The data shall be inspected by following all these steps:
Plot one of the following quantities versus sin ψ : ∆2θφψ{hkl} , 2θφψ{hkl}, dϕψ{hkl},εφψ{hkl} ;
2

Check for non-linear or non-elliptic behaviour (see Figures 2 and 3).
 The net integrated intensities Iϕψ{hkl} after applying the corrections in Annex E.1 shall be plotted
2
versus sin ψ. These intensities are likely to be the same for all ψ-angles recorded for a random, non-
textured specimen. Large changes in intensity are indicative of a highly textured material or coarse
diffracting domains (see Clause 12 and 8.4.3.2).
2
 Plot the line width versus sin ψ. Usually an increase is observed due to defocusing effects. Check
for sudden changes.
8.4.3 Quantitative inspection
8.4.3.1 For a single diffraction line
Diffraction lines can be considered for further analysis if at least the following conditions are fulfilled:
 0.8 times the mean of the experimental peak widths ≤ peak width ≤ 1.2 times the mean of the
experimental diffraction line widths;
 maximum intensity of the diffraction line ≥ 300 counts above background.
Comparison with previous experiments on the same or a similar material is suggested.
8.4.3.2 For the complete set of diffraction measurements
The complete set of diffraction measurements can be considered for further analysis if at least the following
conditions are fulfilled:
{hkl}
Max Iφψ
 For the complete dataset the ratio of the integrated intensity {hkl} shall be smaller than 3 to exclude
Min Iφψ
strongly textured materials.
 The standard deviation of the diffraction line widths shall be less than 10% of the average width.
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Criteria on the uncertainty of the normal stress:
1 1
σ ≥
a) if
(
400 ⋅1 / 2 S 2{hkl } ) then u(σ) shall be ≤
(
1600 ⋅ 1 / 2 S 2{hkl } ) (15a)
1 1 1
σ < {hkl } then u(σ)shall be ≤ (5000⋅1/ 2S {hkl } ) or ≤ 4 σ whichever is the largest .
b) if
( 400 ⋅1 / 2 S 2 ) 2
(15b)
Criteria on the uncertainty of the shear stress:
u(τ) < 1
(10000⋅1/ 2S { } )
2
hkl (16)
where, for formulae (15a), (15b), (16),
u(σ) is the standard uncertainty in the normal stress;
u(τ) is the standard uncertainty in the shear stress;
1 {hkl}
S2 is the elasticity constant of the family of lattice planes{hkl}.
2
9 Report
The experimental conditions, analysis procedures and results shall be recorded.
In particular the following information shall be recorded:
a) A reference to this document.
b) Details of any treatment applied to the specimen prior to stress measurement, which may have altered
the condition of the surface: examples are grinding, polishing (mechanical or electrochemical) and
chemical treatments; if a depth profile of stress is being measured using material layer removal, details of
the method by which material is removed should be reported.
c) Sufficient information about the specimen, e.g. schematic drawing, to locate points and to identify
directions of the measurements
d) Type of equipment including the type of specimen tilting.
e) Technical parameters: current and voltage of the X-ray generator, Kβ filter if used, the values of λ,
1 {hkl}
{hkl}, S2 and S1{hkl}, the reference specimen used, the irradiated area dimension, 2θ range, 2θ step,
2
step counting time, values of φ and ψ.
f) Main information about the fitting routine used, or, if not known, the name and version of the software
package used to analyse the data (method of diffraction line position determination); any variable
parameters used in the peak fitting routine: e.g., constant or sloping background selected, percentage of
the peak used for a centre of gravity calculation, etc.
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g) Method used for residual stress analyses (e.g. biaxial or triaxial method).
h) The results:
1) relevant tables and diagrams;
2) values of the residual stress determined;
3) type and values of uncertainties for the stress values as defined in 8.3.2 and confidence level, if
required.
The report shall at least contain:
i) A reference to this document;
j) Sufficient information about the specimen, e.g. schematic drawing, to locate points and to identify
directions of the measurements;
k) Information about the conformity of the measurement with respect to the standard;
l) X-ray elasticity constants;
m) The results:
1) relevant tables and diagrams,
2) values of the residual stress determined,
3) type and values of uncertainties for the stress values as defined in 8.3.2 and confidence level, if
required.
The report should also contain:

2 2
n) The d-sin ψ or ε-sin ψ - curves and one observed profile; if the diffraction lines recorded are atypical
(because of texture, for example), it may be appropriate to report all diffraction lines along with the results.
o) General information concerning chemical composition, thermal history and any processing performed on
the specimen.
p) If a depth profile of stress is being generated, the depth of each measurement should be recorded relative
to the initial surface position; if depth variation is obtained by changing the incident X-ray wavelength or
intensity, the position of the diffracting gauge volume centroid below the surface should be reported,
along with an indication of how its position has been calculated.
10 Experimental determination of XECs
10.1 Introduction
1 {hkl}
For the correct calculation of residual stresses the X-ray elasticity constants (XECs) S1{hkl} and S2 shall
2
be used. These constants can be found in the literature, calculated through micro/macro mechanical models
or obtained by experiment, as described in this chapter.
The values obtained by experiment are correct for single phase materials. In the case of multiphase materials
a mechanical model is required for an interpretation of the results [15].
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10.2 Loading device
The measurement of the constants requires a specific device to allow the loading of the specimen inside the
diffractometer.
The device shall be designed to apply uniform loads on the irradiated area, taking into account the
measurement geometry. During the loading, the diffractometer measurement area of the loaded specimen
shall be always in the centre of the goniometer.
The load can be pure tension, shearing or bending. Usually four-point bending is recommended.
In order to know the stress, force measurement devices shall be used or strain gauges shall be applied on the
specimen. The loading device shall have been previously calibrated (see 10.3).
Key
S1, S3 specimen coordinate system
L3 laboratory coordinate system
ψ angle between the normal of the specimen and the normal of the diffracting lattice planes.
A applied force
B incident beam
C diffracted beam
D strain gages
Figure 8 — Example of 4 points bending test to determine the X-ray elasticity constant (XEC).
In Figure 8 the stress is tensile and the measurement is done in ω method.
10.3 Specimen
The specimen used for the determination of the XECs should be made of the same material (chemical composition,
microstructure, etc.) as the specimen for residual stress measurements.
It is necessary to accurately control the strain and/or the stress applied. If strain gauges or an extensometer
are used, the macroscopic elasticity constants E and ν are required. If strain gauges are used, one or more
strain gauges shall be applied on the specimen. At least one strain gauge shall be applied parallel to the
specimen longitudinal axis. It is advisable to apply the strain gauges as near as possible to the measuring
area.
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10.4 Loading device calibration and specimen accommodation
The device (for the specimen instrumented with strain gauges) shall be calibrated with a traction standard
testing machine (i.e. a tensile testing machine) or by means of calibrated dead weights. The stresses in the
measurement zone are determined as a function of applied load and geometry. The calibration steps are:
 to perform at least two cycles of loading and unloading from zero to 75% of the yield load (load that would
cause in the specimen a stress equal to the yield limit), in order to verify that the strain-gauge electrical
signal returns to zero at the end of each cycle;
 to perform three cycles of loading and unloading between 5% and 75% of the yield load.
10.5 Diffractometer measurements
The device should be placed at the centre of the diffractometer such that the specimen can be positioned
according to Clause 7.2. Different loads should be applied and for each one the measurement shall be
performed with the specimen oriented in the longitudinal direction.
The applied stress or strain in the measured area shall be evaluated for example by strain gauges.
The measurements shall start from high loads, with measurements performed for decreasing loads to avoid
effects caused by inelastic deformation of the specimen. The minimum number of loading steps shall be five,
regularly distributed between 70% and 5% of the yield load.
10.6 Calculation of XECs
For each step of loading, the average applied stress shall be calculated in order to determine ε φψ :
1 {hkl} R 1
S2{hkl}.τ13 sin2ψ +
R A 2 R
ε φψ = S2 (σ11 −σ33 +σ11 )sin ψ +
2 2
1 {hkl} R
+ ⋅S2 σ33 + S1{hkl} [ Tr(σR ) +σ11A ] (17)
2
2
The elliptical curve (see Eq. 5) ε φψ = a·sin ψ + b·sin(2ψ) + c for each load shall be drawn. The slope ‘a’,
splitting ‘b’ and intercept ‘c’ are evaluated by the least squares method:
1 {hkl} R R A
 a= S2 (σ11 −σ33 +σ11 ) (18a)
2
1
S2{hkl}.τ13 ,
R
 b= (18b)
2
and
1 {hkl} R
⋅S2 .σ33 + S1{hkl}. [ Tr(σ ) +σ11 ]
R A
 c= (18c)
2
Where for formulae (17), (18a), (18b) and (18c)
εφψ{hkl} is the strain in the direction defined by the angles φ and ψ for the family of lattice planes
{hkl};
1 {hkl}
S2 is the elasticity constant of the family of lattice planes {hkl};
2
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σ11Α is the applied stress;

R R R
σ11 , σ22 and σ33 are residual normal stresses;
R
τ13 is the residual shear stress;
R
Tr(σ ) is the trace of residual stresses.
1 {hkl}
The plot of the slope ‘a’ against the applied stress, gives a straight line of slope S2 .
2
The plot of splitting ‘b’ values against the applied stress, shall give a horizontal line of slope 0.
The plot of intercept ‘c’ values against the applied stress, gives a straight line of slope S1{hkl}.
Uncertainties shall be estimated for instance through least squares method and given with the results.
11 Reference specimens
11.1 Introduction
Incorrect alignment of the equipment leads to displacements of the diffraction line.
To verify the alignment the use of a flat specimen without stresses, for example a powder, is suggested.
After alignment verification, measurements on stress-free specimen give an indication of the contributions due
to the not removable misalignment of the goniometer or to electronic or mechanical drifts. Measurements on
stress-reference specimen give a consistent indication on how to calibrate the measurement.
11.2 Stress-free reference specimen
11.2.1 General
The reference powder used shall have a diffraction line with a similar position to that of the specimen under
study (see EN 13925-3).
The powder shall have fine grains and have sufficient intensity of the reflection in all directions. Annealing of
the powder is sometimes useful to improve the line definition.
11.2.2 Preparation of the stress-free specimen
The stress-free reference specimen can be prepared according to EN13925-2:2003 Clause 4.2. In general
such a preparation requires covering a flat, non-crystalline substrate (e.g. a glass plate) with a layer of powder
by:
a) sedimentation from a liquid (e.g. propanol-2);
b) smearing grease in a layer as thin as possible, depositing the powder onto it, pressing it gently, and
carefully shaking off the surplus;
c) deposition on a double sided adhesive film and pressing it gently, and carefully shaking off the surplus;
d) mixing it with grease, depositing the mixture on the glass plate, and levelling it in order to get a flat
surface;
e) mixing it with greasy, liquid glue (without crystalline components) and solvent, depositing the mixture on
the glass plate, and levelling it in order to get a flat surface.
Attention shall be paid to avoiding dissolution of the powder or the substrate, or chemical interaction (such as
polymerisation), which can introduce stresses.
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For the cases a, b, and c:

 adhesion of the powder shall be checked by turning the specimen upside-down and checking for falling
powder;
 it is advised to use a compound with a high average atomic mass in order to have a sufficiently strong
diffraction pattern of the powder and to reduce the intensity diffracted by the substrate through absorption
by the powder.
The use of a thin slab of a single-crystal (e.g. a silicon wafer) as a flat substrate is not recommended because
of the risk of severe damage to the detector by the very strong diffraction of the substrate at some φ, ψ
combinations.
Grease and double-sided adhesive film can yield a significant undulating contribution to the background of the
pattern of the reference powder. Therefore, the thinner the layer of grease or the double sided adhesive film
the better.
The position of the surface of a reference specimen is often adjusted using a mechanical micrometer device,
in which case a thin metal plate of accurately known thickness can be put between the powder and the device
to facilitate accurate positioning of the surface.
11.2.3 Method of measurement
The measurement angles 2θ and ψ used for the reference specimen should be comparable to those used in
the subsequent experiments. The measurement time can be increased to reduce counting statistical errors.
The acceptance of the obtained values shall be made following the criteria stated in Clause 8.4.
11.3 Stress-reference specimen
11.3.1 Laboratory qualified (LQ) stress-reference specimen
11.3.1.1 General
If a laboratory creates a reference specimen which contains a known level of stress it is called a laboratory
qualified (LQ) stress-reference specimen.
11.3.1.2 Manufacturing
The manufacturing process of the reference specimen shall ensure a high homogeneity of microstructure and
a time-constant value of stress.
A simple geometry of the specimen is recommended to ensure quality of the measurement (flatness, low
roughness, etc.). The stress level should be high enough to minimise errors in the measurement. A number of
measurements should be performed by the laboratory on the goniometer which has been carefully aligned
(see Clause 6.5.1). The reference values σref, τref and Lref of the specimen are defined as the averages of
these results. The repeatability r σref, rτref and rLref are equal to 2.8 sσref, 2.8 sτref, 2.8 sLref, where sσref, sτref, and sLref
are the standard deviations on σref, τref and Lref.
11.3.1.3 Evaluation of characteristic parameters
The characteristic parameters are:
 the normal stress value σref and its repeatability rσref ;
 the shear stress value τref and its repeatability rτref ;
 the value of the average width Lref and its repeatability rLref.
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The values of these parameters are obtained according to ISO 5725-1.
The repeatability is obtained according to ISO 5725-2 and the values shall be recorded.
11.3.2 Inter-laboratory qualified (ILQ) stress-reference specimen
An inter-laboratory qualified (ILQ) stress-reference specimen is physically similar to LQ stress-reference

specimens but shall be analysed by several laboratories in order to increase the chances of detecting
systematic errors or improper measurement protocols.
It shall fulfil the basic assumptions of the standard method described in the present document: Weak
crystalline texture, fine grains, flat surface, low roughness, negligible stress or composition gradients in the
depth and along the surface. Furthermore, the mechanical state shall be stable with time. The stress level
should be as high as possible, at least 1 .
(500 12 S 2{hkl } )
It is not necessary to know the chemical composition or the microstructure precisely. The reference values of
the specimen: normal stress σref, shear stress τref and reproducibility Rσ, Rτ and repeatability rσ, rτ values can
be obtained by inter-laboratory round robins involving at least 5 laboratories. Until certified specimens are
commercially available, groups of laboratories can be constituted freely in order to manufacture and
characterise the specimens. Information on the organisation of inter-laboratory round robins can be found in
ISO 5725-2. The computation of repeatability and reproducibility is also described in ISO 5725-2. These are
defined as 2.8 sr and 2.8 sR where sr and sR are standard deviations of the repeatability and reproducibility
respectively.
In the certificate of the specimen the reference values of the specimen shall be indicated along with the
experimental conditions (lattice plane family, radiation and approximate spot size, location of the
measurement area, the ψ values used, XECs, S1 direction, oscillations or masking if any).
12 Limiting cases
12.1 Introduction
The limiting cases are:

 Stress gradients;
 Lattice constants gradient;
 Layer removal (see 5.2.2.2);
 Surface roughness;
 Non-flat surfaces (see 5.1.2);
 Highly textured materials;
 Coarse grain material (see 5.1.4);
 Multiphase materials;
 Overlapping diffraction lines;
 Broad diffraction lines.
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12.2 Presence of a subsurface stress gradient
A strong stress gradient will lead to a curvature of the plot of the lattice spacing (or diffraction line position)
2
versus sin ψ (see Clause 8.4). This curvature is independent of the sign of the ψ values used.
If stress gradients are present, the X-ray diffraction measurement can be used for stress calculations only if:
∂σ 1 1 1
< ⋅ ⋅ (19)
∂Z z 1/2 S2 500
hkl
where
∂σ
is the stress gradient with respect to the distance to the surface of the specimen;
∂Z
z is the penetration of the x-rays;
1 {hkl}
S2 is the elasticity constant of the family of lattice planes{hkl}.
2
The penetration of X-rays can be calculated by formulae reported in Clause 6.3
It is possible to correct the data for the errors caused by the penetration of the X-ray beam, if no depth
measurements are performed and the stress profile is accurately calculated. To minimise gradient effects, and
thus to improve the measurement quality, it is suggested:
 to reduce the X-ray penetration by using a more suitable wavelength,
 to choose a more suitable diffraction angle,
 to use low incidence angles.
12.3 Surface stress gradient
In several cases, regions with high plastic strains may be very confined (plastic strains around inclusions,
cracks or holes, edges of laser treatment or welding, sharp contacts, etc.), and strong gradients are generated.
Thus, in this case the residual stress evaluated by X-ray diffraction depends on the size and the position of the
irradiated area and the assumption of uniform stress holds only if the irradiated area is sufficiently small.
Indeed, if the stress values measured within an area are very different, choosing a large enough irradiated
area may provide a useful “average” surface stress, even if large fluctuations of its local value are present.
But, with the use of a too small diffracting area, an insufficient number of crystallites diffract and the coarse
grain diffraction difficulties may appear [7].
12.4 Surface roughness
12.5 Non-flat surfaces
Curved surfaces lead to too low absolute values of the stress.

The irradiated area should be smaller than 0.4 times the radius of curvature of the analysed surface in the
direction of the stress component to be determined. Beyond this limit, corrections shall be performed [8,9].
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12.6 Effects of specimen microstructure
12.6.1 Textured materials
Texture effects are moderate if the variations of integrated intensity over the whole set of the data fulfil:
{hkl}
Max Iφψ
{hkl} <3 (19a)
Min Iφψ
where
I hkl is the net integrated intensity of the hkl diffraction line.
Otherwise, two effects have to be considered:

 Elastic anisotropy: the relationship between stress and measured strains becomes:
ε φψ = ∑ Fij σ ij , (19b)
i , j=1 to 3
where
εφψ{hkl} is the strain in the direction defined by the angles φ and ψ ;
Fij are called Generalised XEC.
The Fij depend on the Orientation Distribution Function of the material. They can be calculated or determined
experimentally (for details see e.g. [10]).
 Plastic anisotropy: in addition to the effect of macroscopic stresses, the elastic strain of the diffracting
volume contains a term ε φψ
m
related to the accommodation of the local plastic anisotropy:
- ε φψ = Fij σ ij + ε φψ
m
. (19c)
The term ε φψ
m
can cause non-linearity in the ε φψ vs. sin ψ plots. At this time there is no general method to
2
handle the problem.
Measurements on several reflections taking an average of the stress values obtained or establishing the εφψ-
2
sin ψ curve from εφψ values obtained on different reflections may be used.
12.6.2 Multiphase materials
If several phases are present in the specimen, the calculated residual stresses can be attributed, as a first
approximation, to the phase to which the chosen reflection belongs. When the phase is a small percentage or
when its elastic-plastic behaviour is different from that of the pure material, the stress can be greatly different
with respect to the macroscopic stress.
Usually, in these cases there are two ways to obtain the macroscopic stress:
 to measure the strains in all phases;
 to adopt other methods to evaluate the macroscopic stress (by strain gauge, etc...).
With the strains in all phases, the determination of macroscopic residual stresses may present several
difficulties.
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In a single phase material, with the domain size, shear stresses in the planes perpendicular to the specimen
surface may be present (σ13 ≠ σ23 ≠ 0). In the same way, in multiphase materials, accommodation may induce
σ33 ≠ 0 in each phase, especially, when several phase transformations have occurred in the material.
So for the determination of the macroscopic stresses with the classical X-ray method applied on each phase
the volume fraction and the free stress lattice spacing d0 of each phase is required.
In multiphase materials if the grain size is smaller than the penetration depth of the X-rays, then the through
thickness residual stress (σ33) should be taken into account (more precise ref.10).
12.7 Broad diffraction lines
The position of broad diffraction lines is determined with low precision and systematic errors, which may arise
from truncation effects.
In particular, problems can arise when:
 the line width is greater than 1/3 of the angular range of the measurement;
 the difference between the intensities after LP and absorption corrections on the right and left-hand side
of the line is greater than 20% of the intensity of the maximum (see Figure 9).
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Key
H peak height
∆H intensity/asymmetry
A intensity
B acquisition range
Figure 9 — Example of a broad diffraction line that may cause problems of truncation because ∆H >
20% H
In these cases it is suggested:
 to collect a wider 2θ range;
 to change the {hkl} lattice planes;
 to optimise the diffraction line treatment.
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EN 15305:2008 (E)
Annex A
(informative)
Schematic representation of the European XRPD Standardisation Project

TYPES OF ANALYSIS
T General
Standards EN 13925-1 EN 13925-2 prEN 13925-3 Phase Identification
defining the General Basic Characteristics Quantitative Analysis of Phases
C general features of Instruments Macro and micro strani (residual
Principles Procedures
of XRPD stress)
1 NDT Method Texture
EN 1330-11 ……..
3 Terminology ……..
see list in Clause 7 of EN 13925-1
General Principles
8
/
Others (= EN for TYPES OF
ANALYSIS - see Clause 7 of General
W EN 15305 Principles (EN 13925-1):
G Application Residual stress Phase Identification
Standards X-Ray Quantitative Analysis of Phases
1 defining the Macro and micro strains (residual
Testing stress, internal stress etc.)
method of Texture
0 XRPD Technical Specification, Reports,
……..
see also doc. WG10 n.15l Clause 4
Guides, Workshop agreements
Jointed activity CEN ISO/TS CEN ISO/TR 25107

by 21432 Training Syllabus – XRD
Residual stress (Jointed to TC138-AHG8)
TC 138/WG10 Neutrons
and/or other Standard
Protocols and
TCs/Wgs Procedures
Standards, Technical Specification, Reports, Guides Workshop

agreements for specific products in compliance with other TC's as
appropriate
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Annex B
(informative)
Sources of Residual Stress

B.1 General
Residual stresses are generated by any process (mechanical, thermal, chemical), which leads to
inhomogeneous deformation, inhomogeneous volume changes, etc.
B.2 Mechanical processes

 Surface treatments.
 Drawing.
 Rolling.
 Grinding and mechanical polishing.
 Machining.
 Assembling.
B.3 Thermal processes

Residual stresses may arise from thermal gradients as well as from phase transformations, e.g. in the case of
heat-treated steel.
Examples of this are quenching, casting, butt welding, tempering, ageing, etc.
B.4 Chemical processes

Chemical processes, like oxidation, corrosion, electroplating, etc, are sources of residual stress.
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Annex C
(normative)
Determination of the stress state - General Procedure

C.1 General
The mathematical definition used for evaluating deformations is:
 d φψ   sin θ 0 
ε {φψ
hkl}
= ln   = ln  [
 = ln[sin θ 0 ] − ln sin θ φψ ] (C.1)
 d0   sin θ φψ 
The general formula used for the stress tensor calculation in a triaxial stress state is:
ε {φψ
hkl}
= S 2 .
( )
1 {hkl}  σ11 cos 2 φ + σ 22 sin 2 φ + τ12 sin 2φ − σ 33 . sin 2 ψ  {hkl}
()
 + S1 .Tr σ (C.2)
2 + (τ13 cos φ + τ 23 sin φ). sin 2ψ + σ 33 
where for formulae (C.1) and (C.2),
assuming σ33 = 0:
εφψ{hkl} is the strain in the direction defined by the angles φ and ψ for the family of lattice planes {hkl};
d0 is the interplanar distance (d spacing) of a strain free specimen;
dφψ is the interplanar distance (d spacing) of strained material in the direction of measurement
defined by the angles φ and ψ.
θ0 is the Bragg angle associated to d0 ;
θφψ is the Bragg angle associated to dφψaccording to Bragg law (see EN 13925-1:2003, Clause 4);
1 {hkl}
S2 is the elasticity constant of the family of lattice planes{hkl};
2
σ11, σ22, σ33 are normal stress components in the directions S1, S2 and S3;
τ12 is the shear stress within the plane defined by S1 and S2;
Tr(σ) is the trace of the stress tensor : Tr(σ) = Σσii .

Combining these two relations, it is possible to define a procedure to calculate the stress tensor components.
Biaxial and uniaxial stress states are particular cases of the calculation. The procedures to calculate these
stress states are the same, replacing some components σij by a zero value.
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C.2 Using the exact definition of the deformation
C.2.1 General
Replacing the exact definition of ε hkl

φψ (C.1) in relation (C.2), we obtain an expression of Bragg angle θ values
as a function of the stress state.
[ ]
ln sin θ φψ = ln[sin θ 0 ] − S 2 .
( )
1 {hkl}  σ11 cos 2 φ + σ 22 sin 2 φ + τ12 sin 2φ . sin 2 ψ  {hkl}  
 − S1 .Tr  σ  (C.3)
2 + (τ13 cos φ + τ 23 sin φ). sin 2ψ   
where
θ0 is the Bragg angle associated to d0;
θφψ is the Bragg's angle defined in the direction φ and ψ according to Bragg law (EN 13925-1:2003,
Clause 4);
1 {hkl}
S2 is the elasticity constant of the family of lattice planes{hkl};
2
σ11, σ22, σ33 are normal stress components in the directions S1, S2 and S3;
Tr(σ) is the trace of the stress tensor: Tr(σ) = Σσii.
C.2.2 Determination of the stress tensor components
Using
1 {hkl }
aij = − S ⋅ σ ij
2 2
(C.4)
and
K = ln[sin θ 0 ] − S1{hkl}.Tr  σ 
 
(C.5)
 
and with (C.6)
f11 = cos 2 φ ⋅ sin 2 ψ ; f 22 = sin 2 φ ⋅ sin 2 ψ ; f12 = sin 2φ ⋅ sin 2 ψ f 13 = cos φ ⋅ sin 2ψ; f 23 = sin φ ⋅ sin 2ψ
relation (3) can be written :
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3
[ ]
ln sin θ φψ = K + ∑ f ij .aij (C.7)
i, j
Knowing θ φψ values versus fij (5 functions of ψ and φ angles), we can determine the 5 aij constants values and
the constant K value. Linear regression calculation is the most suitable tool for this determination.
Then, the stress is calculated by values which do not depend on θ0 value:

a ij
σ ij = − (C.8)
1 {hkl }
S
2 2
where the symbols in formulae (C.4), (C.5), (C.6), (C.7) and (C.8) are:
σii for the normal stress components (I = 1,2,3);
1 {hkl}
S2 for the elasticity constant of the family of lattice planes {hkl};
2
Tr(σ) for the trace of the stress tensor: Tr(σ) = Σσii;

f11, f22, f12, f13, f23 for the strain coefficients;
θφψ for the Bragg angle defined in the direction φ and ψ according to Bragg law (EN 13925-
1:2003, Clause 4).
C.2.3 Determination of θ and d0
If
 
Tr  σ  = σ11 + σ 22 is known, we can determine θ0, using relation (5). From θ0 d0 is obtained using Bragg’s law.
 
 
The determination of Tr  σ  depends on the type of analysis.
 
This value cannot be determined from a single direction analysis. But, if we consider the stress tensor to be
 
isotropic (σ11 ≈ σ 22 ) , we can write Tr  σ  ≈ 2 ⋅ σ11 .
 
This calculation is not necessary for the determination of stress tensor components, using the general
definition of deformation.
C.3 Using an approximation of the definition of the deformation
C.3.1 General
For historical reasons, a deprecated approximation of the deformation definition may be used:
hkl
θ 0 − θ φψ
ε φψ = (C.9)
tan (θ 0 )
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with
bij = tan (θ 0 ) ⋅ a ij (C.10)
and using the same notations as previously, one can write :
3
θ φψ = K − ∑ f ij ⋅ bij (C.11)
i, j
with K = θ 0 − S1{hkl } ⋅ Tr  σ 
 
 
C.3.2 Determination of the stress tensor components
Knowing θ φψ values versus fij (Five functions of ψ and φ angles), one can determine the five bij constants
values and the constant K value. Linear regression calculation is the most suitable tool for this determination.
Then, stress tensor components are calculated with:
bij
σ ij = − (C.12)
1 {hkl}
S . tan (θ 0 )
2 2
These values depend on θ0 value, which is necessary to calculate the stress tensor components.
This approach induces a systematic error in the stress values.
C.3.3 Determination of θ0 and d0
Sometimes, an approximation of this value is used, such as θ(sin2ψ=0.4). The definition of ()

Tr σ implies:
S1{hkl }
K= .(b11 + b22 ) + θ 0 (C.13)
1 {hkl}
S . tan (θ 0 )
2 2
If at least two perpendicular directions are analysed, then the sum b11 + b22 is known, and θ0 can be
determined resolving the equation (13) by iterative algorithm. (From θ0 d0 is obtained using Bragg’s law.) If
this is not the case, only b11 is known. But, if it is considered that the stress tensor is isotropic (σ11 ≈ σ 22 ) , it is
possible to write b 22 ≈ b11 .
This approach is more complex than the one presented in Annex C.1 and is always an approximation of the
exact θ0 value. It is not to be used.
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Annex D
(informative)
Recent developments
D.1 Stress measurement using two-dimensional diffraction data
If an area detector is used, the basic principle of the ω-tilt, χ- tilt or a combination of the two can be used. In
order to make use of all the information from an area detector in a simple way, it is useful to define an angle γ.
This angle γ is the azimuthal angle on the diffraction cone belonging to a {hkl} reflection as shown in Figure
D.1
Key
L1, L2, L3 laboratory coordinate system
2θ diffraction angle, the angle between the incident and diffracted X-ray beams
X-ray arrow incident beam
γ azimuthal angle
A diffraction plane
B x-ray
Figure D.1 — The geometric definition of diffraction rings in laboratory axes.
The diffraction cone contains far more information than the part of the cone collected in a conventional one-
dimensional measurement.
Diffraction cones from a stress-free polycrystalline specimen are regular cones in which the diffraction angle is
constant. A stress in the specimen distorts the diffraction cones shape so that they are no longer regular
cones. Then the diffraction angle becomes a function of γ, 2θ(γ), and this function is uniquely determined by
the stress tensor and the specimen orientation. This enables stress measurement. The benefit of the 2D
method is that so many data points can be used to calculate stresses that result in a satisfactory
measurement with short data collection time.
The relationship between strain tensor and diffraction cone distortion is defined by the fundamental equation
[11]
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sin θ 0 
f11ε11 + f12ε12 + f22ε 22 + f13ε13 + f23ε 23 + f33ε 33 = ln  (D.1)
 sin θ 
where
εij′s are the strain tensor components in the specimen coordinate system S 1 S 2 S 3 ,
fij′s are strain coefficients determined by the simplified equations in Table D.1.
Table D.1 – Equations for Strain Coefficients fij
f11 = f12 = f22 = f13 = f23 = f33 =
h12 2h1h2 h22 2h1h3 2h2 h3 h32
a = sin θ cos ω + sin γ cos θ sin ω
b = − cos γ cos θ
c = sin θ sin ω − sin γ cos θ cos ω
h1 = a cosφ − b cosψ sin φ + c sinψ sin φ

h2 = a sin φ + b cosψ cos φ − c sinψ cos φ
h3 = b sinψ + c cosψ
NOTE Where {h1 , h2 , h3} are the components of the unit vector of the diffraction vector H hkl expressed in the specimen
coordinates.
The stress tensor can be calculated from the strain tensor by using the general Hooke’s law
σ ij = Cijkl ε kl (D.2)
where
σ ij is the stress tensor;
Cijkl represents the elastic stiffness coefficients in the specimen coordinates. For isotropic materials,
{hkl} 1 {hkl}
there are only two independent elasticity constants, S1 and S2 .
2
We have the equation for stresses:
p11σ11 + p12σ12 + p13σ13 + p22σ22 + p23σ23 + p33σ33 = ln sinθ 0  (D.3)

 sinθ 
where
Pij ′s are stress coefficients
 = 1 S{hkl} f + S1 if i = j
p ij =  12 {2hkl} ij (D.4)
= 2 S2 f ij if i ≠ j
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ln( sin θ 0 sin θ ) determines the diffraction cone distortion at each γ angle which is determined by the
measured function 2θ(γ) for a particular specimen orientation ( ω , ψ , φ ).
The following alternative expressions can be used for the diffraction cone distortion term.
 sin θ 0   λ  (D.4a)
ln   = ln  
 sin θ   2d0 sin θ 
Each diffraction frame corresponds to one specimen orientation ( ω, ψ and φ). The diffraction ring on each
frame is integrated and peak-fitted over a selected number of sections along the ring, so as to obtain a set of
(χ, 2θ) data points representing the 2θ(χ) function. The stress tensor can be determined by fitting the data
points to equation (3) with the least-squares method.
For biaxial stress, the above equation becomes
p11σ 11 + p12σ 12 + p22σ 22 + p phσ ph = ln  λ  (D.5)


 2 d 0′ sin θ 
where
p ph = 12 S {2hkl } + 3 S1{hkl } ,
σ ph
is a pseudo hydrostatic stress component caused by the approximated-spacing d 0′ .
For biaxial stress with shear, we have
p11σ11 + p12σ12 + p22σ 22 + p13σ13 + p23σ 23 + pphσ ph = ln  λ  (D.6)


 2 d 0′ sin θ 
2
The biaxial stress state (Equation D.5) corresponds to the straight line of the d-sin ψ plot. And the biaxial
stress with shear (Equation D.6) is the case when there is a split between the data points in + ψ side and -ψ
side. The general normal stress (σφ) and shear stress (τφ) at any arbitrary given φ angle are given by
σ φ = σ 11 cos2 φ + σ 12 s in 2 φ + σ 22 s in 2 φ (D.7)
τ φ = σ 13 cosφ + σ 23 sin φ (D.8)
In the Biaxial (2D) and Biaxial + Shear (2D) calculation, it is assumed that σ33 is zero so that we can calculate
stress with an approximation of d0 (or 2θ0). Any error in d0 (or 2θ0) contributes only to a pseudo-hydrostatic
term σph. If we use d 0′ to represent the initial input, then the true d0 (or 2θ0) can be calculated from σph with the
following equations:
d 0 = d ′0 exp( p ph σ ph ) (D.9)
or
θ 0 = arcsin [sin θ ′0 exp( − p ph σ ph ) ] (D.10)
D.2 Depth resolved evaluation of near surface residual stress - The Scattering Vector
Method
The scattering vector method [12, 13] is a special X-ray stress analysis (XSA) technique that was developed
for the depth resolved evaluation of near surface residual stress fields. In contrast to the sin² ψ- based XSA
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methods, where the penetration depth zis adjusted by the variation of the inclination angle ψ between the
surface normal and the diffraction vector g hkl, the scattering vector method is based on strain depth profiling
by a specimen rotation η around ghkl at fixed orientations (φ,ψ) of the diffraction vector with respect to the
specimen system. The z -range covered by this rotation corresponds to the difference ∆z = zχ- zωbetween the
penetration depths of the χ-and the ω-method of the conventional XSA.
Because ψ is kept fixed during depth profiling in the ‘scattering vector-’ or ‘η‘ method, the individual stress
tensor depth profiles σij(z), which are coupled in the fundamental equation of the XSA, can be analysed
separately.
The evaluation method is based on the extreme sensitivity of the individual strain profiles εϕψ(hkl, z) with
respect to:
1) strain-free lattice spacing d0(hkl), which can be used as a criterion for a simultaneous
determination of d0(hkl);
2) itself as well as of the σij(z)- profiles.
Therefore, the scattering vector method can be applied to analyse both, biaxial and triaxial residual stress
fields in the near surface zone of polycrystalline materials. In the latter case it yields self-consistently the depth
profiles of the in-plane stresses, σ11(z) and σ22(z), of the stress component σ33(z) normal to the surface, as
well as:
 strain-free lattice spacing d0(hkl). It should be stressed that the method has special preferences for the
analysis;
 of residual stress gradients in strongly textured thin films, because in this case depth profiling can be
performed in;
 intensity poles of the texture and/or at grazing incidence.
D.3 Accuracy improvement through the use of equilibrium conditions for

determination of stress profile
The residual stress fields are linked to incompatible strains generated by inhomogeneous plastic deformation
and are self-balanced over the tested piece and should satisfy the equilibrium equations. So, the tension and
the compression existing at the different points (or depths) of the specimen are not independent one of the
other. The whole set of X-rays diffraction data acquired for different points and inclinations (Φ,Ψ) can be
considered as a one single statistical sampling, and the residual stress and strain profiles can be determined
by a global stress evaluation method [15].
That global method offers several advantages:
1) the errors bars of the evaluated stress profile are greatly reduced;
2) for mechanical resistance approach, that global strain profile determination is the only way for getting
the residual stress fields in F.E.M code;
3) several elements of the residual-stress generation process and elasto-plastic behaviour can be
identified;
4) in the case of a depth profile, the stress redistribution due to the layer removal is taken into account
directly.
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EN 15305:2008 (E)
Annex E
(informative)
Details of treatment of the measured data

E.1 Intensity correction on the scan
E.1.1 General
For the intensity correction the order of corrections shall be reported. The recommended order is:
1) Divergence slit conversion,
2) Absorption,
3) Background removal,
4) Lorentz-Polarisation,
5) K-α2 Stripping.
The instrument contributions (e.g. background and K-Alpha2). shall be included in the calculation of profile
functions that are fitted to the recorded data in order to determine the diffraction line position.
In the report, all the performed correction steps shall be reported and the omitted corrections should be
mentioned too.
E.1.2 Divergence slit conversion
E.1.2.1 General
In Bragg Brentano geometry diffraction patterns are usually recorded using a fixed equatorial divergence slit.
In this case the irradiated area decreases with decreasing diffraction angle. If it is preferred to have a constant
irradiated area, e.g. to ensure that the X-ray beam does not overflow the specimen for all applied angles, then
automatic divergence slits can be used. In data evaluation programs it is usually assumed that the intensities
are measured in Bragg Brentano geometry using a fixed equatorial divergence slit. Consequently, intensities
measured with automatic divergence slits shall be converted to values as if they were measured with fixed
divergence slits under the assumption that the X-ray beam does not overflow the area of the specimen
surface to be probed for all applied angles. This conversion is called a divergence slit conversion.
The conversion formula is
I FDS = C div I ADS (E.1a)
where
IFDS = corrected intensity as if measured with Fixed Divergence Slit;
Cdiv = divergence slit correction factor;
IADS = measured intensity with Automatic Divergence Slit.
The correction factor Cdiv shall be re-evaluated for each measured intensity point.
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If beam overflow occurs intensity corrections are possible, but give only approximate values. Beam overflow
should be avoided if possible.
E.1.2.2 ω method
In the ω method the intensities are usually measured with a fixed equatorial divergence slit and need no
correction.
C div = 1 (E.1b)
In case automatic equatorial divergence slits are applied without beam overflow the intensities shall be
converted to fixed slits intensities.
tan( 12 δ FDS )
C div = 2 R (E.1c)
L ADS sin ω
where
R = radius goniometer;
δFDS = fixed divergence slit angle (full angular range);
LADS = irradiated length;
ω = angle of incidence.
E.1.2.3 χ method
In the χ method, the intensities are usually measured with a fixed axial divergence slit and need no correction.
C div = 1 (E 1d)
Automatic slits are not common with the χ method. In case automatic axial divergence slits are applied without
beam overflow the intensities shall be converted to fixed slits intensities in an appropriate way.
E.1.3 Absorption correction
E.1.3.1 General
For the absorption correction the intensities are assumed to be valid for fixed divergence slits (measured or
corrected) and measured on a thick specimen. For a thick specimen the X-ray beam is fully absorbed by the
analysed part for all applied angles. This condition is adequately fulfilled when the thickness of the analysed
part is at least twice the average information depth, z, as calculated for a thick specimen (see Eqs 9b or 9d).
The correction formula is
I FDS
I Abs −corr = (E.2a)
A
Where
IFDS = corrected intensity as if measured with Fixed Divergence Slit;
A = absorption correction factor.

The absorption correction factor A shall be re-evaluated for each measured intensity point.
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If for a thin specimen partial absorption of the X-ray beam occurs the intensities shall be corrected in an
appropriate way.
E.1.3.2 ω method
For thick specimens the correction factor is:
tan(ω − θ )
A= 1 − (E.2b)
tan θ
where
θ = half of diffraction angle;
(ω-θ) = ω-offset angle.
E.1.3.3 χ method
For thick specimens the correction factor is:
C div = 1 (E.2c)
E.1.4 Background correction
The background is subtracted with:
I Bkg −corr = I meas − I bkg (E.3)
where
Ibkg can be: a) horizontal background (slope = zero);
b) linear background (slope and offset).
The background function is fitted to a number of intensity data points at the extremes of the measurement
range.
The background function fitted and the numbers of intensity data points fitted shall be reported.
The type of background correction should be mentioned (constant background, linear background, spline
approximation…).
E.1.5 Lorentz-polarisation correction
The combined correction for Lorentz and polarisation assumes that the specimen is a polycrystalline material
with random orientation of the crystallites.
The correction formula for the Lorentz-polarisation factor LP is:
I meas
I LP−corr = (E.4a)
LP
where
LP is the combined Lorentz-polarisation factor.
The Lorentz-polarisation factor LP shall be re-evaluated for each measured intensity point.
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1 + Pmon cos 2 2θ
LP = (E.4b)
sin 2 θ cosθ
In the above formulas Pmon describes the extra polarisation owing to the use of a monochromator (in incident
or diffracted beam):
Pmon = cos 2 2θ mon (E.4c)

where
2θ mon = diffraction angle of the monochromator.

If no monochromator is used then
Pmon = 1 (E.4d)
The LP factor used and the value for Pmon shall be reported.
The above combined LP factor holds for diffraction peaks with a low structural broadening, which is not
common in the practice of residual stress analysis. According to Warren & Averbach (1950) referenced by
Delhez, Keijser, Mittemeijer and Rozendaal (1977) the LP factor for profiles with a significant structural
broadening should be:
1 + Pmoncos 2 2θ
LP = (E.4e)
sin 2θ
This last formula should be used for the stress analysis.
E.1.6 K-Alpha2 stripping
The pure K-Alpha1 diffraction pattern is obtained from a K-Alpha1+K-Alpha2 diffraction pattern by means of a
numerical K-Alpha2 stripping procedure. The doublet separation, δR, should be calculated as a 2θ dependent
parameter. See formulae below:
I α 2 (2θ ) = Rint I a1 (2θ − δ R ) (E.5a)
where
Rint ≈ 0.5 (E.5b)
δ R = 2 arcsin( Rwav sin θ α 1 ) − 2θ α 1 (E.5c)
λα 2
Rwav = (E.5d)
λα 1
The value of Rint used shall be reported.
Alpha2 stripping should not be performed if it introduces instabilities in the treatment program, in particular if
there is not enough background available on each side of the line.
E.2 Diffraction line position determination
E.2.1 Centre of Gravity methods
E.2.1.1 Classical Centre of Gravity
The centre of gravity (also called centroid) is calculated to determine the diffraction line position. The centroid
of the profile <2θ> above a threshold value is defined as:
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2θ _ max
∑ 2θ I (2θ )
i = 2θ _ min
i i i
< 2θ >= 2θ _ max

(E.6)
∑ I (2θ )
i
i = 2θ _ min
i
where
2θ is the diffraction angle, the angle between the incident and diffracted X-ray beams;
I(x) is the net intensity.

The threshold value is given as a percentage of the net peak height (i.e. peak height after subtraction of the
background) and marks the starting angle and the end angle at each side of the peak. A too low threshold
makes the method unstable. The recommended threshold is 20%.
E.2.1.2 Centred Centre of Gravity
This is a variant of the classical centre of gravity method.

The iterative sliding centre of gravity method calculates the centre of gravity position using intensities within an
angular range. After the first calculation this range, in terms of a range in 2θ, is centred on the diffraction line
position found in the first step and calculates a new centre of gravity. This step is repeated in an iterative way
until the diffraction line position does not change any more according to a given accuracy value. The initial
angular range is given in terms of an intensity threshold. A too low threshold makes this method unstable. The
recommended initial threshold is 20%.
E.2.1.3 Sliding Centre of Gravity
This is another variant of the classical centre of gravity method. The iterative Sliding Centre of Gravity method
calculates the centre of gravity positions using intensities thresholds between 20% and 80%. For each
Threshold a stress value as well as a corresponding standard deviation is calculated. In a second run, the
centre of gravity positions are weighted with the standard deviation of the corresponding stress value and
averaged. From the final centre of gravity positions a final stress value is calculated.
This method allows to easily detect doubtful measurement and calculation conditions as those conditions
generally cause a large standard deviation of the stress value or a systematic dependency of the stress
values from the intensity threshold. In addition the method provides the automatic refinement of the evaluation
parameters from a statistical point of view [14].
E.2.2 Parabola Fit
The 3-point parabola fit is not recommended.

It is recommended that the parabola function is fit to intensity data points above 85% of the maximum intensity
with a minimum of 5 points.
E.2.3 Profile Function Fit
The definitions of the profile functions are given in EN 13925-2:2003, Annex D.

When using a fitting procedure, it shall be remembered that the more parameters are used, the better the line
description but the greater the risks of instability of the algorithm. Stability problems shall be thoroughly
investigated.
It is recommended to fit a residual background contribution simultaneously with the profile function.
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It is recommended to disable the following fit parameters when they show unstable behaviour: slope of
residual background contribution, asymmetry parameter, and profile shape parameter. In case the profile
shape parameter of the Pearson VII or Pseudo-Voigt function behaves unstable then it is recommended to
use the best fitting profile function with a fixed shape: Gauss, Lorentz, Modified Lorentz, or Intermediate
Lorentz.
E.2.4 Middle of width at x% height method

The width of the diffraction line is determined at x% height of the peak maximum. Straight lines are fitted to the
left and right flank of the peak to determine the width. A smoothing by a sliding polynomial (Stavitsky - Golay)
can also be used. The midpoint of the width is taken as the diffraction line position. The most commonly used
method determines the midpoint of the FWHM (x = 50%). Another common variant uses 2/3 of the height (x =
67%). Other variants are also possible.
E.2.5 Cross-correlation method
The diffraction line position of a diffraction line (Ij) is given relatively to a reference diffraction line (Iref). It is
recommended to use the strongest line of a series of stress measurements as reference line. The cross-
correlation function is defined as:
Fref , j (∆ 2θ ) = ∫ I ref (2θ ) I j (∆ 2θ − 2θ )d (2θ ) (E.7a)
where the maximum of the function Fref,j(∆2θ) gives the diffraction line shift ∆2θref,j. The function Fref,j(∆2θ) is
evaluated for all measurement points of the evaluated diffraction line (Ij) above an intensity threshold. The
recommended threshold is 20% of the net maximum intensity.
The cross-correlation method gives diffraction line shifts only. It is recommended to evaluate the absolute
position of the reference diffraction line with one of the other diffraction line determination methods.
Then the diffraction line position of diffraction line Ij is:
2θ j = 2θ ref + ∆ 2θ j ,max (E.7b)
The method used to determine the diffraction line position of the reference diffraction line shall be reported
unambiguously, together with the function fitted (if any) and the values of the parameters implied.
E.3 Correction on the diffraction line position
E.3.1 General
The diffraction line positions can be optionally corrected for diffraction line shifts caused by remaining
misalignments or the transparency effects. The corrections can be performed on the basis of measured
diffraction line shifts or on the basis of calculated diffraction line shifts. The order of the corrections is not
relevant. The applied corrections shall be reported.
E.3.2 Remaining misalignments
Two misalignment errors are relevant in analysing residual stress measurements: specimen displacement and
incident beam misalignment (equatorial for ω-method and axial for χ-method).
The corrections shall be applied on the diffraction line positions according to the formula:
2θ corr = 2θ meas − ∆ 2θ sp − ∆ 2θ eq − ∆ 2θ ax , (E.8)
with for the ω-method:
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180 2hsp,ω sin θ

∆ 2θ sp = cosθ (E.8a)
π R sin ω
180 2heq sin(ω − θ )

∆ 2θ eq = cosθ (E.8b)
π R sin ω
∆ 2θ ax = 0 (E.8c)
and for the χ-method:

180 2hsp,χ 1
∆ 2θ sp = cosθ (E.8d)
π R cos( χ )
∆ 2θ eq = 0 (E.8e)
180 2hax sin χ

∆ 2θ ax = cosθ (E.8f)
π R cos( χ )
where
2θcorr = corrected diffraction line position
2θmeas = measured diffraction line position
∆2θsp= specimen displacement
∆2θeq= equatorial beam misalignment (only for ω-method)
∆2θax= axial beam misalignment (only for χ - method).
E.3.3 Transparency correction
E.3.3.1 General
The diffraction line shift due to the transparency effect is usually calculated. It requires first the calculation of
the information depth (= weighted mean penetration depth) for each tilt.
The correction shall be applied on the diffraction line positions for each diffraction line according to the
formula:
2θ corr = 2θ meas − ∆ 2θ tr , (E.9a)
E.3.3.2 ωmethod
For thick specimens the information depth is:
sin 2 θ − sin 2 (ω − θ )
z= (E.9b)
2µ sin θ cos(ω − θ )
Then the diffraction line shift (in degrees) is:
− 180 2 z sin(θ ) cos(θ )

∆ 2θ tr = (E.9c)
π R sin ω
where
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µ is the linear attenuation coefficient;
θ is the Bragg angle; this is the angle between the diffracting lattice planes and the incident beam;
(ω-θ) is the offset angle;
z is the information depth;
R is the diffractometer radius.

E.3.3.3 χ method
For thick specimens the information depth is:
sin θ cos χ
z= (E.9d)
2µ
Then the diffraction line shift is:
− 180 2 z cos θ
∆ 2θ tr = (E.9e)
π R cos χ
where
µ is the linear attenuation coefficient;
θ is the Bragg angle, this is the angle between the diffracting lattice planes and the incident beam;
χ is the tilt angle;
z is the information depth;
R is the diffractometer radius.

The transparency correction is usually negligible. It plays a role when the linear absorption coefficient, µ, is
-1
smaller than 200 cm . For ceramics, oxides, light metals and polymers using Cr, Co or Cu radiation this is the
case and for metals and hard metals too when Mo radiation is used.
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Annex F
(informative)
General description of acquisition methods

F.1 Introduction
In the main text of the normative, only three acquisition methods are described, the ω method, the χ method
and the modified χ method: The two first because they are widespread in both industrial and university
laboratories and the third one because it is often used on portable goniometers. However, other methods exist
that can be used for specific purposes. The aim of the present annex is to provide a general description of
acquisition methods followed by applications to various methods used for X-ray stress analysis.
An acquisition method is defined by the set of orientations taken by the specimen with regard to the incident
beam and the diffracted beams during the acquisition. The orientation of a solid is defined by a set of three
angles that correspond to its three rotational degrees of freedom.
In X-ray stress analysis, the most fundamental set of three angles is (Φ, Ψ, η) where Φ and Ψ define the
r r
measurement direction n and η is a rotation angle around n . However, this set of angle is not always
convenient because, in general, they do not correspond to the angles of the goniometer. The purpose of the
present annex is to give the relation between the two sets of angles in the case of a Euler cradle using the
angles (ϕ, χ, ω). A similar approach can be given for any other kind of cradle such as a kappa cradle.
F.2 Definitions
Two orthonormal reference systems are defined:

(S , S , S )
r r r
The first one, called specimen reference system, is noted by: 1 2 3
r

S 3 is taken normal to the surface of the specimen and directed towards the outside.
r
 S1 is in the plane of the surface and freely chosen by the operator. It is customary to choose it parallel to
a physically meaningful direction such as the rolling direction, the machining direction, the welding
direction, etc.
( )
r r r r
 S 2 is taken so that the S1 , S 2 , S 3 system is direct.
 If the surface of the specimen is curved, the system is chosen with respect to the tangent plane at the
point of measurement.
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Key
(G , G , G )
r r r
1 2 3 goniometer reference system
θ azimutal angle on the diffraction cone
A diffracted beam (y ≠ 0)
B for (y ≠ 0)
C incident beam
D for y = 0
E diffracted beam (y=0)
Figure F.1 — Definition of the diffraction angles 2θ and γ (right)
(G , G , G )
r r r
The second one, called the goniometer reference system, is noted by: 1 2 3
r
 G 1 is taken parallel to the incident X-ray beam and directed in the propagation direction of the photons;
r
 G 2 is taken parallel to the axial direction of the goniometer;
( )
r r r r
 G 3 is taken so that the G1 , G 2 , G 3 system is direct.
In the reference (starting) position, the two systems are superposed. The data acquisition is defined
completely by the orientation of the two systems. Three groups of angles can be defined:
The first group is called the sampling angles, noted Φ, Ψ, η (capital phi, psi, eta) and is related to the
mechanical state of the specimen at a given penetration depth. These angles define completely the orientation
(S , S , S ) .
r r r
of the specimen and are useful if one works in the system 1 2 3
 Φ and Ψ are the extensometric angles and they are called respectively azimuth and tilt angles. They
(S , S , S ) , the direction of measurement of the elastic strain ε
r r r
define, in the system 1 2 3 ΦΨ . This direction is
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r
described by a unit vector noted n . For a given crystallographic plane family, Φ and Ψ enable to sample
different crystallites that produce the diffraction peak.
r
 η defines a rotation around n . A variation of η will cause a variation of the penetration depth (information
depth). It will also cause a variation of ε ΦΨ only if there are stress gradients along the depth of the
specimen. For given diffraction conditions and extensometric angles, η enables to sample different
depths below the surface of the specimen.
The second group is called the 3 goniometer angles ϕ, χ, ω (small phi, chi, omega) and they are used to
(G , G , G ). From the
r r r
orientate the specimen on the goniometer, they are useful if one works in the system 1 2 3
reference position, the specimen is brought into its measurement orientation by three successive rotations. It
should be noticed that the order of the three rotations is important.
r
 A rotation by ϕ around − G 3
r
 A rotation by χ around G 1
r
 A rotation by ω around − G 2
Key
(S , S , S )
r r r
1 2 3 reference system
X incident beam
open circle diffracted beam
black dot bisector of the two beams
A specimen
B X-ray beam source
C detector
Figure F.2 - Reference position (χ = ϕ = ω = 0)
Reference position (χ = ϕ = ω = 0) the incident beam is parallel to the surface of the specimen and the two
(S , S , S ) (G , G , G )
r r r r r r
reference systems 1 2 3 and 1 2 3 are superposed. Perspective drawing (left) and
stereographic representation for 2θ = 156° (right).
The third group is called the diffractometric angles θ and γ (theta, gamma) and they define the direction of the
diffracted beam:
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 θ is called the Bragg angle and the angle between the incident beam and the diffracted beam is 2θ.
r
 In a polycrystalline specimen, the diffracted beams form a cone of axis G 1 and γ defines the position of
one diffracted beam in the cone. The measurement direction is the bisector of the incident and diffracted
beams.
In the following section, an acquisition method is described by giving the expressions of Ψ and Φ as a function
of the goniometer angles (ϕ, χ, ω) and of the diffraction angles (θ, γ). The expressions of the penetration depth
is given as a function of the diffraction angles and either with the sampling angles (η, Ψ, θ, γ) or with the
goniometer angles (χ,ω, θ, γ). It can be noted that the penetration depth does not depend on angles ϕ or Φ for
a specimen with a flat surface.
A particular acquisition method is obtained from the general method by setting some angles at a given fixed
value.
F.3 Description of the various acquisition methods
F.3.1 General method
The expressions of Ψ and Φ are:

Ψ = ArcCos(cos γ cos θ cos χ cos ω + sin γ cos θ sin χ + sin θ cos χ sin ω) (F.1)
and:
Φ = ϕ + ∆ϕ

  − sin γ cos θ cos χ + cos γ cos θ sin χ cos ω + sin θ sin χ sin ω  (F.2)
∆ϕ = ArcTan cos γ cos θ sin ω − sin θ cos ω

  
where:
Φ and Ψ are respectively the azimuth angle, the tilt angle;
γ is the azimuthal angle on the diffraction cone belonging to a {hkl} reflection;
θ is the Bragg angle;

r
χ is the specimen orientation in the direction G1 ;
r
ω is the specimen orietation in the direction − G2 ;
r
ϕ is the specimen orientation in the direction − G3 of the goniometer system;
r
∆ϕ is the additional rotation of the specimen in the direction − G3 .
All the acquisition modes with a 0D (punctual) or 1D (position sensitive) detector can be described by γ = 0.
When a 2D detector is used, angle γ is necessary to describe the variations of Φ and Ψ along the portion of
the Debye ring captured by the detector. The penetration depth can be given with the sampling angles:
cos 2 Ψ sin 2 θ − sin 2 Ψ cos 2 θ sin 2 η

z= (F.3)
2µ sin θ cos Ψ
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or with the goniometer angles :
cos χ sin ω  sin 2θ cos γ cos χ cos ω + sin 2θ sin γ sin χ − cos 2θ cos χ sin ω 
z=   (F.4)
µ  sin 2θ cos γ cos χ cos ω + sin 2θ sin γ sin χ − cos 2θ cos χ sin ω + cos χ sin ω 
where
z is the penetration depth.

F.3.2 Omega (ω) method
This is an acquisition mode that can be achieved with a basic 2 circles (ω ; 2θ) powder diffractometer and a
0D or 1D detector. In this case γ = 0, χ = 0 and η=π/2. From formulae (E.1) to (E.4), it gives:
Ψ = ω − θ
 (F.5)
Φ = ϕ
with a penetration depth:
sin 2 θ − sin 2 Ψ sin 2 θ − sin 2 (ω − θ)

z= = (F.6)
2µ sin θ cos Ψ 2µ sin θ cos(ω − θ)
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X
S2
ç
S1
Key
(S , S , S ) and (G , G , G ) superposed reference systems

r r r r r r
1 2 3 1 2 3
L3 is normal to the diffracting {hkl} lattice planes

2θ the diffraction angle; this is the angle between the incident and diffracted X-ray
beams
ω the angle between the incident X-ray beam and the specimen surface at χ = 0
ψ the angle between the normal of the specimen and the normal of the
diffracting lattice planes
X the incident beam direction
° (open circle) the diffracted beam
• (black dot) the bisector of the incident and diffracted beams
Figure F.3 - Perspective drawing of the omega method for Φ=0 and Ψ=0 or Ψ=−45° (left). Stereographic
representation for Φ=0 and three values of Ψ : -45°, 0, +45° (right).
F.3.3 Chi (χ) method
This mode is obtained by using the χ rotation of a Eulerian cradle to achieve the Ψ tilt and a 0D or 1D
detector. In this case γ = 0, ω = θ and η = 0. From formulae (E.1) to (E.4), it gives:
Ψ = χ
 (F.7)
Φ = ϕ + π / 2
with a penetration depth:
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sin θ cos Ψ sin θ cos χ

z= = (F.8)
2µ 2µ
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X
X X
X X X X X
S2
ç ç ç ç ç ç
ç
ç
S1
Key

r r r r r r
1 2 3 1 2 3
L3 is normal to the diffracting {hkl} lattice planes.

2θ the diffraction angle. this is the angle between the incident and diffracted X-ray
beams
χ The angle χ rotates in the plane perpendicular to that containing ω and 2θ.

Figure F.4 - Perspective drawing of the chi method for Φ=90° and Ψ=0 or Ψ=+60° (left). Stereographic
representation for Φ=90° and 8 values of Ψ : −45°, 0, 15°, 30°, 45°, 60°, 75° et 90°. (right).
F.3.4 Combined tilt method (also called scattering vector method)
These are general acquisition modes that give penetration depths and optical aberrations that are in between
the omega and chi modes. From arbitrary values of χ, ϕ and ω, the expressions of Ψ and Φ are given from
formulae (E.1) and (E.2):
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Ψ = sign( ω − θ) ArcCos(cos χ cos(ω − θ) )


  sin χ  (F.9)
Φ = ϕ + ∆ϕ with ∆ϕ = ArcTan  tan( ω − θ) 
  
For given values of Φ and Ψ there is an infinite set of (χ, ϕ, ω) values which can be obtained by rotating the
r
incident and diffracted beams around the measurement direction n by an angle η. The penetration depth is
given from formulae (E.3) and (E.4) with γ = 0 :
cos 2 Ψ sin 2 θ − sin 2 Ψ cos 2 θ sin 2 η

z= (F.10)
2µ sin θ cos θ
cos χ sin( 2θ − ω) sin ω

z= (F.11)
2µ sin θ cos(θ − ω)
By varying η from zero (χ method) to 90° (ω method), the penetration depth can be varied without changing Φ
and Ψ.
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X X X S2
X
X
ç
ç ç
ç ç
S1
Key
(S , S , S ) and (G , G , G )
r r r r r r
1 2 3 1 2 3 superposed reference systems

beams
Figure F.5 - Perspective drawing of the combined method for Φ = 70°, Ψ = 60° and η = 22.5° (left).
Stereographic representation for Φ = 70°, Ψ = 60° and 5 values of η : 0, 22.5°, 45°, 67.5° and 90°..
F.3.5 Modified chi method
This mode is used on some portable goniometers with two detectors placed symmetrically on each side of the
incident beam. Angle ω is set equal to π/2 so that at χ = 0 the incident beam is normal to the specimen
surface. The χ and ϕ rotations are used to vary the measurement direction. The use of two detectors allows to
2
compensate for the ∆ϕ so that Ψ ≈ χ with minor systematic errors on the sin Ψ slope (which can be easily
corrected). For detector 1, angle γ is equal to zero and for detector 2, angle γ is equal to π.
Ψ = ArcCos(cos χ sin θ)

Detector 1 :  π  −1  (F.12)
Φ = ϕ + 2 + ∆ϕ with ∆ϕ = ArcTan  sin χ tan θ 
  
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Ψ = ArcCos(cos χ sin θ)

Detector 2 :  π  1  (F.13)
Φ = ϕ + 2 + ∆ϕ with ∆ϕ = ArcTan  sin χ tan θ 
  
As can be seen, the two ∆ϕ compensate each other. Thus, when the strains measured by the two detectors
are averaged they disappear. The measured strain (equation (5) of main text) can thus be written:
ε φψ = 12 S{2hkl} sin 2 θ sin 2 χ (σ φ − σ 33 ) + 12 S{2hkl} sin 2 θ sin 2χ τ φ + K (F.14)

where:
K = S1{hkl}Tr (σ) + 12 S{2hkl} (sin 2 θ σ 33 + cos 2 θ σ φ+ π / 2 ) (F.14bis)
This equation can be used exactly like equation (5) by replacing Ψ by χ, and, in the end divide the obtained
2
normal stress and shear stress values by sin θ. The penetration depth is identical for the two detectors:
cos ψ ( 2 sin 2 θ −1 ) cos χ (1 − cot an 2 θ)

z= = (F.15)
2 µ sin 3 θ 2µ
It should be noted that the diffracting crystallites sampled by the two detectors are not the same. This can
cause some problems in the case of textured specimens or large crystallite size specimens.
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ç
ç
ç
ç
ç ç ç
X X X X X X XS2
ç ç ç
ç ç
ç
ç
S1
Key

r r r r r r
1 2 3 1 2 3

beams
Ψ the angle between the normal of the specimen and the normal of the
D1 detector 1
D2 detector 2
Figure F.6 - Perspective drawing of the modified chi method (left). Starting position (up) with ω = 90°, ϕ
r
= χ = 0. Position for χ = 60° et ϕ = 0 (down), which corresponds to a measurement in direction S 2 i.e.,
after averaging the strains obtained from the two detectors, to the direction Φ = 90°. Stereographic
representation for 2θ = 140°, ω = 90°, ϕ = 0 and 7 values of χ : 0, 15°, 30°, 45°, 60°, 75° and 90° (right).
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It can be noticed in Figure F.6 that the values of Ψ are always greater than the corresponding values of χ. For
detector 1, Ψ varies from 20° to 90° while Φ varies from 0 to 50°. Fir detector, Ψ varies from 20° to 90° while Φ
varies from 180° to 130°.
F.3.6 Low incidence method
This mode is used to achieve shallow penetration depth and wide irradiated surfaces. The idea is to set ω at a
fixed value α typically 2 to 5°. The χ and ϕ rotations are used to vary the measurement direction. A 0D
detector with long Soller slits is used to reduce optical aberrations so γ = 0 :
Ψ = ArcCos(cos χ cos(α − θ) )

  sin χ  (F.16)
Φ = ϕ + ∆ϕ with ∆ ϕ = ArcTan  
  tan( α − θ) 
The penetration depth is given directly from equation (E.11) by setting ω = α :
cos χ sin( 2θ − α) sin α
z= (F.17)
2µ sin θ cos(θ − α)
Another way to define this mode is to keep constant at a given value α the angle between the surface of the
specimen and the incident beam, i.e. to keep constant the value of sinα = cosχ sinω.
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XX XXX
X
ç ç
ç ç
ç ç ç
S2
S1
Key

r r r r r r
1 2 3 1 2 3

beams
α is a fixed value of ω typically comprised between 2 and 5 degrees.
Figure F.7 - Perspective representation of the low incidence mode (left). On top, starting position with
ω = α, χ = ϕ = 0. Down, position for χ = 60° and ϕ = 0. Stereographic representation for ω = α = 5°, 2θ =
120°, ϕ = 0 and 7 values of χ : -75°, -60°, -30°, 0, 30°, 60°, 75°.
It can be noticed in Figure F.7 that, in this configuration, Ψ varies from 55° to 82° while Φ varies
simultaneously from 146° to 214°.
F.3.7 Modified omega method
This mode is used on some portable goniometers. It is very similar to an omega mode but the Ψ0 angle that is
set on the goniometer is taken between the normal to the specimen surface and the incident beam.
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 π
Ψ = Ψ0 + − θ
 2 (F.18)
Φ = ϕ
with a penetration depth given by (F.6).
Key
(S1, S2, S3) specimen coordinate system
(G , G , G )
r r r
1 2 3 goniometer reference system
(L1, L2, L3) laboratory coordinate system.
2θ the diffraction angle; this is the angle between the incident and diffracted X-ray beams
Figure F.8 - Perspective drawing of the modified omega method.
By comparing with Figure F.3, it is clear that the two methods only differ through the origin in Ψ.
F.3.8 Use of a 2D (area) detector
The use of a 2D detector allows to acquire a whole section of the diffraction cone (of the Debye ring), i.e. a
whole range of γ values. According to equations (F.1) and (F.2), it corresponds to a whole range of Ψ and Φ
values. Theoretically, one acquisition is sufficient to obtain enough information for calculating some stress
components however in practice the acquisition range in Ψ is too small to give reasonable accuracies. At least
a second acquisition for another value of χ, ω or ϕ is advised. The relevant equations for this method are (F.1)
to (F.4), i.e. the general equations.
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Key

r r r r r r
1 2 3 1 2 3

2θ diffraction angle; this is the angle between the incident and diffracted X-ray
beams
ω angle between the incident X-ray beam and the specimen surface at χ =0
X incident beam direction
° (open circle) diffracted beam
• (black dot) bisector of the incident and diffracted beams
A for y = 0
B for y ≠ 0
Figure F.9 - Perspective representation of a possible set-up to work with a 2D detector for ω = θ = 70°
and χ = ϕ = 0 (left).
In Figure F.9 a plane detector is shown, but cylindrical detectors also exist. The detector acquires a section of
the diffraction cone for γ varying from - 45° to + 45°. On the right, stereographic representation for ω = θ = 70°
and ϕ = 0 and 9 values of γ : -60°, -45°, -30°, -15°, 0, 15°, 30°, 45°, 60°. On top, representation for χ = 0 : it
can be seen that Ψ varies from 0 to 20° while Φ varies simultaneously from - 90° to + 90°. Down,
representation for χ = 40°, Ψ varies from 22° to 58° while Φ varies from 90° to 115°.
F.4 Choice of Φ and Ψ angles
When measurements are performed in only one direction Φ, the minimum number of tilt angle Ψ is 2 for a
biaxial stress state and 3 for a triaxial stress state. However, due to sampling effects linked to the
microstructure of the material, it is generally acknowledged that this minimum is actually not sufficient. That is
why the present standard recommends four or five 5 tilts for the biaxial case and seven for the triaxial case.
The same question arises for tensor analysis. The minimum number of (Φ, Ψ) couples is six, taken in, at least,
three independent Φ directions. Several ways are possible to choose the Φ directions. One of the most
common is to take:
Φ = 0, 45° and 90° with positive and negative Ψ values (F.19)
However, as it can be seen on a stereographic representation, this is not the best sampling possible, i.e. the
directions are not spread as uniformly as possible in the whole available solid angle. If three Φ directions are
79
BS EN 15305:2008
EN 15305:2008 (E)
chosen, a better choice is:

Φ = 0, 60° and 120° with positive and negative Ψ values (F.20)
Whether (F.19) or (F.20) is chosen is the same problem as for rosette strain gauges: if the principal stresses
are known before the measurement, (F.19) is easier to use, but if they are not known, (F.20) will be more
accurate.
More than three directions can be chosen. It is necessary to check the consistency of the results, to calculate
the uncertainty on the stress components and it will increase the overall accuracy of the measurement. It is
thus advised to use at least four Φ directions. If n is the number of directions, the Φ values can be separated
by:
∆Φ = 180°/n (F.21)
For instance, for five Φ directions, the Φ values can be : 0, 36°, 72°, 108° and 144°.
Figure F.10 - Stereographic representations of different choices for the Φ directions
In Figure F.10 on the left, three directions are chosen according to (F.19). On the middle, three directions are
chosen according to (F.20) or (F.21). On the right, five directions are chosen according to (F.21).
F.5 The stereographic projection
The stereographic projection is a useful tool to represent accurately directions (crystallographic directions,
measurement directions, diffracted and incident beams…) emanating from a specimen which is assumed
(S , S , S ). The direction ofrinterest
r r r
punctual and located at the origin O of the reference system 1 2 3 intersects a
sphere of radius R centred on O. The intersection point is then projected on to the (S , S ) plane of the
r
1 2
specimen surface. The projection issues from a centre H which is the south pole of the sphere.
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BS EN 15305:2008
EN 15305:2008 (E)
Key
H the south pole of the sphere
Φ the angle between a fixed direction in the plane of the specimen and the projection in that plane
of the normal to the diffracting lattice planes
Ψ the angle between the normal of the specimen and the normal of the diffracting lattice planes
r
Figure F.11 - Example of a stereographic representation of a direction n described by angles Φ = 60°
and Ψ=45° (right).
In Figure F.11 the angle Φ can be read directly on the projection and angle Ψ can be read along a radius of
the projection circle. On the perspective drawing on the left, only one eighth of the sphere is represented.
r r
For instance, let’s take a direction n described by the two angles Φ and Ψ. The straight line directed by n
( )
r r
intersects the sphere at point N. The line (HN) intersects the plane S1 , S 2 at point N’ which is the
r
stereographic projection of n (black dot on Figure F.10). The coordinates of N’ in the reference system
( )
r r
S1 , S 2 are :
 Ψ
x = R cos Φ tan 2 
  
 (F 22)
 y = R sin Φ tan Ψ 
 2
To make the use of a stereographic projection easier, it is graduated every 10° in Φ and every 10° in Ψ. The
r
S3 direction (corresponding to Ψ=0) is at the centre of the projection circle while the direction for which Ψ =
90° are located on the external edge of the circle. Thus, on Figure F.10, the values of Φ (60°) and Ψ (45°) can
be read directly and unambiguously. The incident beam (X mark) and the diffracted beam (white dot) can also
be represented clearly as compared with a perspective drawing that would be confusing.
81
BS EN 15305:2008
EN 15305:2008 (E)
Annex G
(informative)
Normal Stress Measurement Procedure" and "Dedicated Stress

Measurement Procedure
G.1 Introduction
This annex introduces concepts for a Dedicated Stress Measurement Procedure. It is to be verified and it shall
become normative in the future. i
G.2 General
G.2.1 Introduction
Two stress measurement procedures are defined and described that conform to this standard and that yield
results (stress values) of which it is allowed to be denoted as "stress measurements according to this
standard":
a) the Normal Stress Measurement Procedure that shall be applied to specimens with an unknown stress
state and to specimens where the stress state is not assessed or proven;
b) the Dedicated Stress Measurement Procedure that can be applied to series of very similar specimens
(routine analyses) e.g. with the purpose of reducing the measurement effort.
The Dedicated Stress Measurement Procedure is introduced to enable qualified and standardized stress
measurements for e.g. quality control and stress mapping, and it shall guarantee a proven and tractable one
to one relationship between the results obtained with the Normal Procedure and the Dedicated Stress
Measurement Procedure.
G.2.2 Normal stress measurement procedure for a single specimen
The normal stress measurement procedure is described in Clauses 7.1 to 7.4
G.2.3 Dedicated Stress Measurement Procedure for very similar specimens
Specimens are regarded here as "very similar" if the differences between their stress states (not the stress
values), their chemical and phase compositions, their texture, their microstructure are expected to be
insignificant for the stress values to be determined.
For a series of such specimens a laboratory can define and describe a Dedicated Stress Measurement
Procedure. In order to conform to this standard such a Dedicated Stress Measurement Procedure shall be
validated through the execution of the Normal Procedure as well as the Dedicated Stress Measurement
Procedure. The validation procedure requires that:
1) the validation measurements shall be performed on several specimens of the series to establish the
allowable range of stress values;
2) the equipment shall be aligned and validated/qualified according to Clauses 6.5 and 6.6 before
starting the validation of the Dedicated Stress Measurement Procedure as well as before starting the
measurement on the series of specimens;
82
BS EN 15305:2008
EN 15305:2008 (E)
3) it proves that the value obtained by the Dedicated Stress Measurement Procedure is appropriate and
sufficient for the purpose, i.e. that the reduction of measurement effort is justified.
The procedure shall define (i) quantitatively the acceptable deviations from the expectations of the
2
intermediate results (e.g. the linearity of εφψ versus sin ψ plots, the shear stress value, the peak width) that are
relevant to the stress determination and (ii) the procedure to be followed if unacceptable deviations are
observed.
If the Dedicated Stress Measurement Procedure obeys the above, then the stress results obtained using that
procedure are accepted as conforming to this standard.
83
BS EN 15305:2008
EN 15305:2008 (E)
Bibliography
[1] CEN ISO TS 21432, Non-destructive testing - Test method for measurement of residual stress by
neutron diffraction
[2] MOORE, M.G., EVANS, W.P., Mathematical correction for stress in removed layers in X-ray diffraction
residual stress analysis, SAE Transactions, vol. 66, 1958, pp. 340-345; Handbook on Techniques of
Residual Stresses Measurement”, SEM (American Society for Experimental Mechanics), J. Lu and
M.R. James editors, 1996)
[3] E1237-93(2003), Standard Guide for Installing Bonded Resistance Strain Gages, ASTM International
[4] PFEIFFER, W., A new intensity and background correction procedure for Ω-diffractometers.
Materialprűfung 37, 7-8, s292-295 (1995)
[5] FRANÇOIS, M. et al., Reference specimens for x-ray stress analysis: the French experience,
Metrologia 41 (2004) pp. 33-40
[6] FRANÇOIS, M., LEBRUN, J.L., X-ray stress determination on materials with large size crystallites-
theoretical approach, Proc. of the 3rd European Conf. on Residual Stresses (ECRS 3), 4-6 Nov. 1992,
Frankfurt, Germany
[7] HENNION, V., SPRAUEL, J.M., and MICHAUD., H., Contribution to residual–stress evaluation in high-
stress-gradient zones by X-ray diffraction, J.Appl.Cryst. (2000). 33, 26-34
[8] FRANÇOIS, M., DIONNET, B., SPRAUEL,J.M., NARDOU, F., The influence of cylindrical geometry on
X-ray stress tensor analysis, part I, general formulation, J. of Applied Crystallography, vol. 28, 1995,
pp. 761-767
[9] DIONNET, B., FRANÇOIS, M., SPRAUEL, J.M., NARDOU, F., The influence of cylindrical geometry
on X-ray stress tensor analysis, part II: applications, J. Appl. Cryst. (1999) 32, pp. 883-891
[10] HAUK, V., BEHNKEN, H., REIMERS, W., PFEIFFER, W., GENZEL, Ch., et al., Structural and
Residual Stress Analysis by Non destructive Methods, Elsevier, 1997, ISBN 0 444 824 766
th
[11] HE, B. B., The 20 ASM Heat Treating Society Conference Proceedings, Vol.1, pp 408-417, St. Louis,
Missouri, 2000
[12] GENZEL, Ch., A Self-Consistent Method for X-Ray Diffraction Analysis of Multiaxial Residual Stress
Fields in the Near Surface Region of Polycrystalline Materials. I. Theoretical Concept. J. Appl. Cryst.,
32 (1999), pp. 770 - 778
[13] GENZEL, Ch., BRODA, M., DANTZ, D., REIMERS, W., A Self-Consistent Method for X-Ray Diffraction
Analysis of Multiaxial Residual Stress Fields in the Near Surface Region of Polycrystalline Materials. II.
Examples, J. Appl. Cryst., 32 (1999), pp. 779 - 787
[14] SPRAUEL, J.M. and MICHAUD, H., Global X-ray method for determination of stress profiles, Materials
Sciences forum Vols. 404-407 (2002), pp. 19-24
[15] PFEIFFER, W. (1994), The role of the peak location method in X-ray stress measurement. Proc. of the
Fourth Int. Conf. on Resid. Stresses, SEM, Bethel, CT, USA, pp. 148-155
[16] ISO 1993, Guide to the Expression of Uncertainty in Measurement (Geneva, Switzerland: International
Organisation for Standardisation)
[17] KIRKUP, L., A guide to GUM, Eur. J. Phys. 23 (2002), pp. 483–487
84
BS EN 15305:2008
EN 15305:2008 (E)
[18] HAUK, V., BEHNKEN, H., REIMERS, W., PFEIFFER, W., GENZEL, Ch., et al., Structural and
Residual Stress Analysis by Non-destructive Methods, Elsevier, 1997, ISBN 0 444 824 766
[19] NOYAN, I.C., and COHEN, J.B., Residual Stress: Measurement by Diffraction and Interpretation,
Springer-Verlag, 1987
[20] Handbook of Residual Stress and Deformation in Steel, ASM International, 2002
[21] ASTM E915-96, Standard test method for verifying the alignment of x-ray diffraction instrumentation
for residual stress measurement, ASTM International, 2002
[22] ASTM E1426-98, Standard test method for determining the effective elastic parameter for x-ray
diffraction measurements of residual stress, ASTM International, 2003
[23] LODINI, A., PERRIN, M., ed., Analyse des contraintes résiduelles par diffraction des rayons X et des
neutrons, INSTN/CEA, 1996
[24] LU, J., RETRAINT, D., Review of recent developments and applications in the field of X-ray diffraction
for residual stress studies, Journal of Strain Analysis for Engineering Design, v 33, n 2, 1998, pp. 127-
136
[25] FITZPATRICK, M.E., FRY, A.T., HOLDWAY, P., KANDIL, F.A., SHACKLETON, J. and SUOMINEN, L.,
NPL Good Practice Guide No. 52: Determination of Residual Stresses by X-ray Diffraction, March
2002, ISSN 1368-6550
[26] SCHOLTES, B., Verfahrensbeschreibung - Röntgenographische Ermittlung von Spannungen -

Ermittlung und Bewertung homogener Spannungszustände in kristallinen, makroskopisch isotropen
Werkstoffen, Arbeitsgemeinschaft Wärmebehandlung und Werkstofftechik e.V. (AWT), 2000
[27] EN 1330-11, Non-destructive testing – Terminology – Terms used in X-ray diffraction from
polycrystalline and amorphous materials
[28] CEN ISO/TR 25107, Non-destructive testing – Guidelines for NDT training syllabuses (ISO/TR
25107:2006)
85
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15305:2008
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BRITISH STANDARD BS EN 15305:2008

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

This British Standard is the UK implementation of EN 15305:2008.

This British Standard Amendments/corrigenda issued since publication

ISBN 978 0 580 55634 0

EUROPEAN STANDARD EN 15305

Non-destructive Testing - Test Method for Residual Stress

This European Standard was approved by CEN on 4 July 2008.

EUROPEAN COMMITTEE FOR STANDARDIZATION

Management Centre: rue de Stassart, 36 B-1050 Brussels

8.2.2 Intensity corrections ...........................................................................................................................30

E.1.6 K-Alpha2 stripping...............................................................................................................................59

 EN 13925-1, General principles;

 Lattice constants gradient ;

 Non-flat surfaces (see 5.1.2);

 Highly textured materials;

 Coarse grained material (see 5.1.4);

 Overlapping diffraction lines;

for the determination of repeatability and reproducibility of a standard measurement method

3 Terms, definitions and symbols

3.1 Terms and definitions

3.2 Symbols and abbreviations

 {hkl Family of crystal lattice planes defined by the indices h, k and l.

 εφψ Strain measured in the direction defined by the angles φ and ψ.

 d0 Interplanar distance (d spacing) of a strain free specimen.

 dφψ Interplanar distance (d spacing) of strained material in the direction of measurement

 (S1, S2, S3) Specimen coordinate system.

 (L1, L2, L3) Laboratory coordinate system.

 σii Normal stress components (i = 1,2,3).

 τij Shear stress components (i ≠ j ; i,j = 1,2,3).

 Z Distance to the surface of the specimen.

 z X-ray penetration depth.

 LP The Lorentz Polarization factor.

 A The Absorption factor.

 ILQ Inter-Laboratory Qualified (used in connection with stress-reference specimen).

 LQ Laboratory Qualified (used in connection with stress-reference specimen).

 σcert Certified normal stress value of the ILQ stress-reference specimen.

 τcert Certified shear stress value of the ILQ stress-reference specimen.

 σref Normal stress value of the LQ specimen.

 τref Shear stress real value for the LQ specimen.

Determined Normal stress value of the stress-reference specimen.

 τdetermined Shear stress value determined for the stress-reference specimen.

 u( ) Standard uncertainty in the normal stress.

 u(τ) Standard uncertainty in the shear stress.

 Rσcert, Rτcert Reproducibility of the normal stress and shear stress.

 λ Wavelength of the X-rays used.

 Tr(σ) Trace of the stress tensor: Tr(σ) = Σσii.

 I hkl Net integrated intensity of the hkl diffraction line.

 XECs X-ray elasticity constants.

 sr and sR Standard deviations of the repeatability and reproducibility.

 σφ Normal stress value in a direction defined by the angle φ.

 τφ Shear stress value in a direction defined by the angle φ.

NOTE Elasticity constant is also referred to as elastic constants.

4.1 General principles of the measurement

S1, S2 axes in the plane of the specimen; S1 is defined by the operator

Figure 1 — Orthogonal coordinate systems relevant to XRD stress determination

σ φ = [σ 11 cos 2 φ + σ 22 sin 2 φ + τ 12 sin 2φ ] (1b)

τ φ = [τ 13 cos φ + τ 23 sin φ ] (1c)

σφ normal stress component in a direction defined by the angle φ;

σ11, σ22 normal stress components in the directions S1, S2;

τφ shear stress value in a direction defined by the angle φ.

ε φψ {hkl } ≅ −cot (θ 0 )∆θφψ (2c)