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Metal materials - Quantitative phase analysis - Value K method of X-ray diffraction
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YB/T 5320-2006: PDF in English (YBT 5320-2006) YB/T 5320-2006
YB
FERROUS METALLURGY INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
(Adjusted from GB/T 5225-1985)
Metal materials - Quantitative phase analysis - "Value
K" method of X-ray diffraction
ISSUED ON: JULY 27, 2006
IMPLEMENTED ON: OCTOBER 11, 2006
Issued by: National Development and Reform Commission of PRC
Table of Contents
1 Principles ... 3
2 Requirements and preparation of specimens... 4
3 Test instruments and test conditions ... 6
4 Test procedure and result calculation ... 7
Appendix A (Supplementary) ... 9
Appendix B (Supplementary) ... 12
Additional information ... 14
(hjkjlj) - The cumulative intensity of diffraction lines of the reference material
from the crystal plane (hjkjlj), in the reference specimen;
Wr - The weight of the reference substance, after adding the powder to be
tested into the reference substance;
Wo - The weight of the powder to be tested, when adding the powder to be
tested into the reference substance;
- The weight of the reference substance, in the reference specimen;
- The weight of the powder to be tested, in the reference specimen.
The characteristic of this method is to calculate the first AND finally
determine the Xa.
Note: The reference specimen refers to the specimen, which is prepared when the
value is calculated.
2 Requirements and preparation of specimens
2.1 Sampling
2.1.1 Weighing
When weighing the sample, the relative deviation of the weight shall not exceed
0.1%.
2.1.2 Reference materials and reference specimens
2.1.2.1 Selection of reference materials
The principles for selecting reference materials are:
a. During the test, its physical and chemical properties are stable AND not
easy to deliquesce;
b. The intensity of the diffraction line, which is used for measurement, shall
be strong; its peak position is close to the measured diffraction line of the
phase to be measured, without overlapping each other; meanwhile it is
not interfered by other diffraction lines;
c. The linear absorption coefficient and particle radius of the reference
material shall be as close as possible to the phase to be measured. The
The overall stability of the diffractometer1 is better than 1%.
3.2 Test conditions
3.2.1 Scanning speed
It should choose 0.5 degrees per minute or 0.25 degrees per minute.
3.2.2 Time constant
It should choose 2 s or 4 s accordingly.
3.3 Requirements for diffraction peak shape
The peak height shall be 4 times larger than the fluctuation range of the
background;
The peak height should be about 4 times the half-height width.
4 Test procedure and result calculation
Before the quantitative determination, the intensity of the diffraction lines of the
reference specimen and the mixed specimen shall first be calibrated with the
JCPDS standard card, to check whether the reference material and the phase
to be measured have a preferred orientation. If there is a preferred orientation,
it shall prepare the specimen again, to improve or eliminate the preferred
orientation, as much as possible. When the preferred orientation is not serious,
follow Appendix B to make corrections.
4.1 Determination of value of reference specimen
4.1.1 To calculate the pure phase to be measured of the value, it shall first
carry out qualitative analysis of the X-ray diffraction line, to check the purity;
there shall be no impurity diffraction lines.
4.1.2 For the pure reference material selected according to 2.1.2, it shall check
its purity according to 4.1.1.
4.1.3 Mix samples according to 2.1.1 and 2.1.2, respectively.
4.1.4 Prepare samples according to 2.1.4 and 2.2.
1 The comprehensive stability of this standard instrument refers to the relative standard deviation σ-1 of
the measured diffraction line intensity value within 8 hours, when measuring the diffraction intensity
once every 10 min, on the same diffraction surface of the same specimen, under the same test
conditions.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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