Designation: E 915 – 96 (Reapproved 2002)

Standard Test Method for

Verifying the Alignment of X-Ray Diffraction Instrumentation
for Residual Stress Measurement1
This standard is issued under the fixed designation E 915; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope ment. This method is suitable for application to conventional

1.1 This test method covers the preparation and use of a flat diffractometers or to X-ray diffraction instrumentation of either
stress-free test specimen for the purpose of checking the the diverging or parallel beam types.3, 4
systematic error caused by instrument misalignment or sample 3.2 Application of this test method requires the use of a flat
positioning in X-ray diffraction residual stress measurement, or specimen of stress-free material that produces diffraction in the
both. angular region of the diffraction peak to be used for stress
1.2 This test method is applicable to apparatus intended for measurement. The specimen must be sufficiently fine-grained
X-ray diffraction macroscopic residual stress measurement in so that large numbers of individual crystals contribute to the
polycrystalline samples employing measurement of a diffrac- diffraction peak produced. The crystals must provide intense
tion peak position in the high-back reflection region, and in diffraction at all angles of tilt, c, which will be employed (see
which the u, 2u, and c rotation axes can be made to coincide Note 1).
(see Fig. 1). NOTE 1—Complete freedom from preferred orientation in the stressfree
1.3 This test method describes the use of iron powder which specimen is, however, not critical in the application of the technique.
has been investigated in round-robin studies for the purpose of
verifying the alignment of instrumentation intended for stress 4. Procedure
measurement in ferritic or martensitic steels. To verify instru- 4.1 Instrument Alignment:
ment alignment prior to stress measurement in other alloys, 4.1.1 Align the X-ray diffraction instrumentation to be used
base metal powder having the same crystal structure as the for residual stress measurement in accordance with the instruc-
alloy should be prepared in similar fashion and used to check tions supplied by the manufacturer. In general, this alignment
instrument alignment at the appropriate diffraction angle. must achieve the following, whether the u, 2u, and c axes are
1.4 This standard does not purport to address all of the variable or fixed (see Fig. 1):
safety concerns, if any, associated with its use. It is the 4.1.1.1 The u, 2u, and c axes shall coincide.
responsibility of the user of this standard to establish appro- 4.1.1.2 The incident X-ray beam shall be centered on the c
priate safety and health practices and determine the applica- and 2u axes, within a focusing range, which will conform to the
bility of regulatory limitations prior to use. desired error and precision tolerances (see sections 5 and 6).
4.1.1.3 The X-ray tube focal spot, the c and 2u axes, and the
2. Referenced Documents receiving slit positioned at 2u equals zero degrees shall be on
2.1 ASTM Standards: a line in the plane of diffraction. Alternatively, for instrumen-
E 11 Specification for Wire-Cloth Sieves for Testing Pur- tation limited to the back reflection region, the diffraction angle
poses2 2u shall be calibrated.
4.1.1.4 The proper sample position shall be established,
3. Significance and Use using whatever means are provided with the instrument, such
3.1 This test method provides a means of verifying instru- that the surface of the sample is positioned at the u and c axes
ment alignment in order to quantify and minimize systematic , within the focal distance range which will conform to the
experimental error in X-ray diffraction residual stress measure- desired error and precision tolerances (see sections 5 and 6).
4.1.1.5 The angle c must be determined accurately.
1
This test method is under the jurisdiction of ASTM Committee E28 on
3
Mechanical Testing and is the direct responsibility of Subcommittee E28.13 on Hilley, M. E., Larson, J. A., Jatczak, C. F., and Ricklefs, R. E., eds., Residual
Residual Stress Measurement. Stress Measurement by X-ray Diffraction, SAE J784a, Society of Automotive
Current edition approved Apr. 10, 1996. Published June 1996. Originally Engrs., Inc., Warrendale, PA (1971).
4
published as E 915 – 83. Last previous edition E 915 – 90. “Standard Method for X-Ray Stress Measurement,” Committee on Mechanical
2
Annual Book of ASTM Standards, Vol 14.02. Behavior of Materials, The Society of Materials Science, Japan, (20 April 1973).

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 E 915 – 96 (2002)

FIG. 1 X-Ray Diffraction Stress Measurement Geometry and Angles Defined

4.2 X-Ray Optics: 4.4 Stress-Free Specimen Preparation:

4.2.1 When the Ka characteristic radiation doublet is used 4.4.1 A permanent stress-free specimen may be prepared by
for stress measurement, it is desirable to select incident and mounting the powder on the face of a microscope slide or in a
receiving X-ray beam optics that will produce maximum shallow powder tray (of the type used for powder diffraction
separation of the Ka1 − Ka2 doublet. Perform stress measure- work on a diffractometer) using a 10 % solution of nitrocellu-
ments on the stress-free specimen employing the Ka1 diffrac- lose cement5 diluted with acetone as a suitable amorphous
tion peak at all c angles investigated. Because resolution of the binder. Place several drops of the solution on a clean micro-
Ka doublet may vary with the angle c, and because some scope slide or in a sample tray, and sprinkle the powder into the
instrumentation may be incapable (due to fixed X-ray optics) of binder. The powder may be spread and leveled with a second
obtaining resolution of the doublet, care must be taken not to microscope slide. When a uniform flat surface has been
resolve the doublet at some c angles while blending the produced by alternately wetting with the binder solution and
doublet into a single peak at other c angles. wiping with a second slide, set the specimen aside and allow it
4.3 Selection of Powder for a Stress-Free Iron Specimen: to dry for several hours. Excess amounts of the binder may
4.3.1 Use iron powder with a particle size greater than 1 µm cause it to peel away from the surface of the microscope slide.
(4 3 10− 5 in.) (See Note 2.) Rewetting of the surface with acetone and redrying may
NOTE 2—Annealed armco iron powder of <45 µm (325 mesh) has been
eliminate this difficulty. Make the surface of the specimen as
found suitable. flat as possible so that the specimen surface is clearly defined.
4.4.2 A temporary specimen may be rapidly prepared using
4.3.2 Annealing of the powder in vacuum reduces diffrac- petroleum jelly as an amorphous binder. Place a small quantity
tion peak width, thereby increasing diffraction peak resolution. of petroleum jelly on the face of one microscope slide and
This is generally desirable (see Note 3). Powders in the form of press it against a second slide to extrude the petroleum jelly
plastically deformed filings may be used, but will produce into a uniform flat film. Remove the second microscope slide
broader diffraction peaks. In the event that an instrument with a wiping action taking care to keep the surface layer of
incapable of resolution of the Ka1 − Ka2 doublet is being petroleum jelly thin and flat. Holding the petroleum jelly-
employed, it may be desirable to deliberately obtain plastically coated slide at a steep angle to a vertical line, sprinkle the iron
deformed powders which insure that partial resolution of the powder from a sufficient height above the slide so that the
Ka doublet does not occur. Extremely fine powders have also powder strikes the coated surface and either adheres or is
been shown to produce line broadening, sufficient to suppress deflected away. Do not allow the powder to pack and build up
resolution of the Ka doublet. on the surface.
NOTE 3—It may be advantageous to anneal an oxide-forming powder in
a reducing atmosphere rather than in vacuum to avoid problems from
surface contamination. It is not necessary to anneal ceramic powders since
these materials do not tend to show line broadening from plastic 5
Duco Cement available from DuPont Co., Wilmington, DE 19898 has been
deformation. found suitable. Paraffin wax may also be used.

2
 E 915 – 96 (2002)
4.4.3 The surface area of the powder must be of sufficient the event that the mean differs from zero by more than 14 MPa
size to intersect the entire incident X-ray beam at all c angles (2.0 ksi), repeat 4.1 and 4.5.
to be used during stress measurement. 5.2 Random Error:
4.5 Instrument Alignment Check: 5.2.1 Experience has shown that the standard deviation of
4.5.1 Position the stress-free specimen on the X-ray diffrac- the five measurements should be within approximately 6.9
tion apparatus (see 4.1.1.4). In the event that a mechanical gage MPa (1.0 ksi). In the event that the standard deviation of the
which contacts the surface of the specimen is used for five measurements exceeds 14 MPa (2.0 ksi), the stress-
specimen positioning, a thin metal shim may be placed in front measurement technique employed and the instrumentation
of the powder surface to protect it. Place this gage against the should be investigated for sources of random error affecting the
face of the metal shim, and adjust the positioning to account for measurement precision. Random error due to counting statis-
the inclusion of the shim in front of the gage such that the tics may result from failure to take sufficient time during the
surface of the powder is at the correct distance from the measurement to obtain accurate intensity information, and thus
reference point of the gage for stress measurement. to accurately determine the diffraction peak positions. Methods
are available3 for estimating the standard deviation of the
NOTE 4—Failure to place the powder surface directly over the center of
rotation of the c and 2u axes induces a systematic specimen displacement measured stress due to the errors involved in counting and
error. curve fitting to determine peak positions. Mechanical sources
of error such as loose bearings and ways in the apparatus may
4.5.2 Without adjusting the specimen position, perform five
result in significant random error.
successive stress measurements using the method and correc-
tion procedures normally employed for the instrument. To 6. Precision and Bias
avoid systematic error in the verification process when Ka 6.1 The precision of this method will be dependent upon the
radiation is being used, care must be taken to either completely type of X-ray diffraction instrumentation employed and the
split or blend the Ka1 − Ka2 doublet (see 4.2). methods of data reduction used in stress measurement. The
NOTE 5—Values for accuracy and precision of the various angles and preliminary results of round-robin investigations using this
displacements are not specified herein. These may be considered to be met method indicate that instrument alignment within 14 MPa (2.0
collectively when overall measurement errors and tolerances are within ksi) (see 5.1) can be achieved for both standard diffractometers
those specified in Sections 5 and 6. and two types of X-ray diffraction instrumentation designed for
stress measurement in the back reflection region only. Instru-
5. Calculations and Interpretation of Results
mental precision measured by this method (see 5.2) has been
5.1 Systematic Error: found to be less than 66.9 MPa (1.0 ksi).
5.1.1 Reduce the X-ray diffraction data obtained from the 6.2 The accuracy of this method is considered to be absolute
five measurements in whatever manner is normally employed because the specimen is stress-free. Deviation of results
for the X-ray diffraction instrumentation in use, and include all obtained in performing this method, provided the specimen has
corrections normally applied to raw X-ray diffraction data. been properly prepared and maintained, can be attributed to the
Calculate the simple arithmetic mean and standard deviation instrumentation under investigation.
about the mean for the five measurements. If the mean value is
within 14 MPa (2.0 ksi) of zero, the instrument and specimen- 7. Keywords
positioning gage can be considered to be properly aligned. In 7.1 alignment; residual stress; x-ray diffraction

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