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GB/T 17360-2020 (GBT17360-2020)

GB/T 17360-2020_English: PDF (GBT 17360-2020, GBT17360-2020)
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BASIC DATA
Standard ID GB/T 17360-2020 (GB/T17360-2020)
Description (Translated English) Microbeam analysis -- Method of quantitative determination for low contents of silicon and manganese in steels using electron probe microanalyzer
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard N53
Classification of International Standard 71.040.99; 77.040.30
Word Count Estimation 14,195
Date of Issue 2020-06-02
Date of Implementation 2021-04-01
Drafting Organization Institute of Metal Research, Chinese Academy of Sciences
Administrative Organization National Microbeam Analysis Standardization Technical Committee (SAC/TC 38)
Proposing organization National Microbeam Analysis Standardization Technical Committee (SAC/TC 38)
Issuing agency(ies) State Administration for Market Regulation, National Standardization Administration

Standards related to: GB/T 17360-2020

GB/T 17360-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.99;77.040.30
N 33
Replacing GB/T 17360-2008
Microbeam analysis - Method of quantitative
determination for low contents of silicon and
manganese in steels using electron probe
microanalyzer
ISSUED ON: JUNE 02, 2020
IMPLEMENTED ON: APRIL 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
Introduction ... 4 
1 Scope ... 5 
2 Normative references ... 5 
3 Terms and definitions ... 6 
4 Basic principle ... 6 
5 Instruments and auxiliary equipment ... 7 
6 Reference material ... 7 
7 Sample preparation ... 7 
8 Test conditions ... 8 
9 Establishment of calibration curve ... 9 
10 Measurement of test sample ... 14 
11 Measurement of uncertainty ... 14 
12 Test report ... 15 
Annex A (informative) Examples of determination of manganese content in steel
by calibration curve method and evaluation of uncertainty ... 16 
Annex B (informative) Example of test report format for determination of
manganese content in steel by calibration curve method ... 19 
Bibliography ... 21 
Microbeam analysis - Method of quantitative
determination for low contents of silicon and
manganese in steels using electron probe
microanalyzer
1 Scope
This Standard specifies the calibration curve method that uses electron probe
to determine the contents of silicon and manganese in carbon steel and low
alloy steel (iron mass fraction is greater than 95%).
This Standard is applicable to electron probe spectrometers, not to energy
spectrometers. Scanning electron microscope with spectrometer can refer to
this Standard as reference.
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.
GB/T 4930, Microbeam analysis - Electron probe microanalysis - Guidelines
for the specification of certified reference materials (CRMs)
GB/T 13298, Inspection methods of microstructure for metals
GB/T 15074, General guide of quantitative analysis by EPMA
GB/T 15247-2008, Microbeam analysis - Electron probe microanalysis -
Guidelines for determining the carbon content of steels using calibration
curve method
GB/T 20725, Electron probe microanalysis guidelines for qualitative point
analysis by wavelength dispersive X-ray spectrometry
GB/T 21636, Microbeam analysis - Electron Probe Micro Analysis (EPMA) -
Vocabulary
manganese) Kα line intensity ratio k and the silicon (or manganese) mass
fraction w. As long as the intensity ratio of the silicon (or manganese) Kα line is
measured on the test sample under the same test conditions, the mass fraction
of silicon (or manganese) in the sample can be obtained from the calibration
curve.
5 Instruments and auxiliary equipment
5.1 Electron probe analyzer.
5.2 Metallographic microscope and sample preparation device.
5.3 Ultrasonic cleaning device.
6 Reference material
6.1 The establishment of a calibration curve for the determination of silicon (or
manganese) content REQUIRES at least 5 alloy reference substances with
different silicon (or manganese) content and the content range covering the
mass fraction of silicon (or manganese) element in the test sample. In addition,
pure silicon (or manganese) reference materials are required.
6.2 For the selected series of alloy reference materials, in addition to meeting
the requirements of GB/T 4930, the matrix composition shall be close to the
chemical composition of the test sample. When the alloy elements other than
silicon (or manganese) in the test sample do not have spectral interference and
other factors that affect the quantitative analysis results of silicon (or
manganese), Fe-Si (or Fe-Mn) solid solution can be selected as reference
material. When there are other alloy elements that interfere with the measured
spectrum of silicon (or manganese) in the test sample, the selected reference
material shall also contain the same amount or content of these alloying
elements.
7 Sample preparation
7.1 The analysis surface of the sample shall be ground and polished. The
operation method can be in accordance with GB/T 13298. Observe under a
metallurgical microscope with a magnification of 200 ~ 500 times. There shall
be no grinding defects such as wear marks on the surface of the sample.
7.2 Depending on the situation, the surface of the test sample and the reference
material can be treated with the same degree of light corrosion, or neither is
corroded.
Reasonably set the pulse height analyzer parameters to eliminate the
interference of high-order diffraction lines.
9 Establishment of calibration curve
9.1 According to the requirements of GB/T 20725, conduct qualitative analysis
of the test sample first. According to the analysis results, select the appropriate
alloy reference material combination.
9.2 Under the same test conditions, on the series of alloy reference materials
with different silicon content and the pure silicon reference materials,
sequentially measure the peak intensity IP and background intensity IB of silicon
Kα. The determination of background intensity is usually shown in Figure 1. At
the appropriate positions BG-, BG+ on both sides of the spectrum peak (pay
attention to avoid interference lines and absorption edges), respectively
measure X-ray counting. Then use linear interpolation to calculate the
background intensity. For nonlinear background, special background models
are required. Using linear interpolation will bring additional errors.
The intensities of the alloy reference material and pure silicon reference
material silicon Kα peak can be calculated by formula (1) and formula (2)
respectively:
Where,
Ii(Si) -- The intensity of the ith alloy reference material silicon Kα line (after
background correction);
-- The peak intensity of the silicon Kα line measured on the ith alloy
reference material;
-- The background intensity of the ith alloy reference material silicon Kα
line;
Ipure(Si) -- The intensity of pure silicon reference material silicon Kα line (after
background correction);
-- The peak intensity of the silicon Kα line measured on a pure silicon
reference material;
Where,
wi -- The mass fraction of the ith data point element;
-- The arithmetic mean of data column wi;
ki -- The intensity ratio of the characteristic X-ray of the ith data point;
-- The arithmetic mean of data column ki;
n -- The total number of data points used to build the calibration curve.
The correlation coefficient R of the calibration curve shall meet: R≥0.99,
otherwise all links in the test process need to be checked. Ensure that the test
requirements are met. And re-determine.
10 Measurement of test sample
Use the same test conditions as when establishing the calibration curve.
Measure and calculate the intensity ratio k of the silicon (or manganese) Kα line
in the test sample. Substitute formula (7) to get the mass fraction of silicon (or
manganese) in the sample.
11 Measurement of uncertainty
Typical factors affecting the measurement of uncertainty include changes in
environmental conditions, instruments, analytical testing procedures, and the
state of the sample itself. Operator factors shall also be considered. For detailed
sources of uncertainty, refer to Annex C of GB/T 17359-2012[4].
The uncertainty of the results measured by the calibration curve method can be
evaluated by the method given in Annex A of GB/T 15247-2008. The
repeatability of the test method shall be obtained by repeating the measurement
of the same area in the sample in a short period of time by the same operator
on the same instrument and the same test conditions. The reproducibility of the
testing method shall be determined by repeating tests performed by different
operators at different times.
For the application example of determination of manganese content in steel by
calibration curve method and evaluation of uncertainty, see Annex A.
...