Skip to product information
1 of 6

PayPal, credit cards. Download editable-PDF & invoice In 1 second!

GB/T 17360-2020 English PDF (GBT17360-2020)

GB/T 17360-2020 English PDF (GBT17360-2020)

Regular price $225.00 USD
Regular price Sale price $225.00 USD
Sale Sold out
Shipping calculated at checkout.
Quotation: In 1-minute, 24-hr self-service. Click here GB/T 17360-2020 to get it for Purchase Approval, Bank TT...

GB/T 17360-2020: Microbeam analysis -- Method of quantitative determination for low contents of silicon and manganese in steels using electron probe microanalyzer

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.
GB/T 17360-2020
GB
NATIONAL STANDARD OF THE
PEOPLE 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) K?? line intensity ratio k and the silicon (or manganese) mass fraction w. As long as the intensity ratio of the silicon (or manganese) K?? 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 K??. 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 K?? peak can be calculated by formula (1) and formula (2) respectively:
Where,
Ii(Si) -- The intensity of the ith alloy reference material silicon K?? line (after background correction);
-- The peak intensity of the silicon K?? line measured on the ith alloy
reference material;
-- The background intensity of the ith alloy reference material silicon K?? line;
Ipure(Si) -- The intensity of pure silicon reference material silicon K?? line (after background correction);
-- The peak intensity of the silicon K?? 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) K?? 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.

View full details