GB/T 16597-2019 PDF English
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| GB/T 16597-2019 | English | 260 |
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Analytical methods of metallurgical products - General rule for X-ray fluorescence spectrometric methods
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| GB/T 16597-1996 | English | 479 |
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Analytical methods of metallurgical products. General rule for X-ray fluorescence spectrometric methods
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GB/T 16597-2019: Analytical methods of metallurgical products - General rule for X-ray fluorescence spectrometric methods
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT16597-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 10
Replacing GB/T 16597-1996
Analytical methods of metallurgical products – General rule
for X-ray fluorescence spectrometric methods
Issued on. JUNE 04, 2019
Implemented on. MAY 01, 2020
Issued by. State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Terms and definitions... 5
4 Fundamentals... 10
5 Instruments... 11
6 Reagents and materials... 20
7 Preparation method of sample... 20
8 Qualitative analysis... 21
9 Semi-quantitative analysis... 22
10 Quantitative analysis... 22
11 Common analysis software... 26
12 Safety precautions... 26
13 Recording and presentation of measurement results... 26
1 Scope
This standard specifies the general requirements for quantitative analysis of elements
by X-ray fluorescence spectrometry, including terms and definitions, basic principles,
instruments, reagents and materials, preparation methods of samples, quantitative
analysis, safety precautions, records and expression of measurement results.
This standard applies to wavelength dispersive and energy dispersive X-ray
fluorescence spectrometers, to measure the element composition and element content
in various materials. It can be used for qualitative and quantitative analysis of constant
and trace of all elements from 4Be to 92U in the periodic table, in addition to H, He, Li,
for wavelength dispersive and energy dispersive X-ray fluorescence spectrometers,
which use X-ray tubes as excitation sources. The mass fraction range of the analyzed
elements. 0.0001% ~ 100%.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6379.2 Accuracy of measurement methods and results (trueness and precision)
- Part 2.Basic methods for determining the repeatability and reproducibility of
standard measurement methods
JJG 810 Wavelength dispersive X-Ray fluorescence spectrometers
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
X-ray intensity
The count of intensity in X-ray fluorescence spectroscopic analysis per unit time,
usually represented by I.
3.2
Energy resolution
The ratio -- of the half height width of the pulse height distribution TO the average
pulse height, expressed as a percentage.
3.3
Background
The continuum superimposed on the analytical line, which is mainly due to the
scattering of incident radiation by the sample.
3.4
Analytical line
The characteristic spectral line, whose intensity needs to be measured to determine
the content of the analyzed element accordingly.
Note. In X-ray fluorescence spectroscopic analysis, the characteristic spectral lines with
high intensity, less interference, low background are generally selected as the analytical
lines.
3.5
Interference line
Spectral line, that overlaps or partially overlaps with the analytical line, thereby
affecting the accurate measurement of the analytical line intensity.
4 Fundamentals
4.1 Basic principles of wavelength dispersive X-ray fluorescence spectroscopy
The atoms of elements are excited by high-energy radiation, to cause the transition of
electrons in the inner shell, at the same time emit X-rays with a certain characteristic
wavelength.
4.2 Basic principles of energy dispersive X-ray fluorescence spectroscopy
The analysis sample is excited by the excitation source, to emit characteristic X-rays.
An X-ray detector, which has a certain energy resolution, is used to detect various
energy characteristic X-rays, which are emitted by the sample.
5 Instruments
5.1 Composition of instrument
5.1.1 Wavelength dispersive X-ray fluorescence spectrometer
The schematic diagram of the wavelength dispersive X-ray fluorescence spectrometer
is as shown in Figure 2.
5.1.2 Energy dispersive X-ray fluorescence spectrometer
5.1.2.1 Instrument composition. The composition of the energy dispersive X-ray
fluorescence spectrometer is as shown in Figure 3; the whole set consists of four parts.
Gas replacement device Cooling device High voltage power supply
5.1.3 X-ray generator
The X-ray generator is composed of X-ray tube, high-voltage power supply, and
controller.
5.1.5 X-ray analysis target
5.1.5.1 Commonly used targets for wavelength dispersive X-ray fluorescence
analyzers
5.1.7 Counting-recording systems
Select the desired pulses from the output pulses of the detector to count; display and
record it. It is composed of a pre-positioned amplifier, a single-channel wave height
analyzer, a scaler, a timer, and a counting rate meter. The functions of each part are as
follows.
5.1.8 Data processing system
The computer and its software are used to correct the X-ray intensity AND convert it
into the content of the analyzed elements.
5.1.9 Ventilation mechanism
In order to reduce the absorption of long-wave X-rays by the atmosphere, there shall be
a vacuum system or a helium replacement system, as well as a device to maintain its
pressure stably.
5.2 Selection of instrument parameters
5.2.1 Optical path medium
It is divided into three different optical path media. air, vacuum, helium. Light elements
shall be measured in vacuum media. Liquid and wet powder samples shall be measured
in a helium system, because of the evaporation of water; however, only elements after
fluorine can be measured.
5.2.3 Commonly used analyzing crystals and their scope of application
Commonly used analyzing crystals and their scope of application are listed in Table 3.
5.2.4 Recommended instrument parameters
The recommended instrument parameters for wavelength dispersive X-ray fluorescence
analysis are as shown in Figure 6.
5.3 Placement of instrument
In order to keep the X-ray fluorescence spectrometer in normal working condition, the
following points shall be paid attention to, when placing the instrument.
5.4 Calibration of instrument
In addition to doing daily maintenance and correcting the drift of the instrument with
standardized samples, the technical indicators of the instrument shall be verified
regularly every year, including precision, stability, X-ray counting rate, detector
resolution, counting linearity of the instrument.
6 Reagents and materials
6.1 Lithium tetraborate (Li2B4O7). Before use, ignite at 600 °C for 4 hours; cool and
seal for later use; it is superior grade or analytical grade.
6.2 Lithium metaborate (LiBO2). before use, ignite at 600 °C for 4 hours; cool and seal
for later use; it is superior grade or analytical grade.
6.6 Lithium bromide (LiBr). Superior grade or analytical grade.
6.7 Ammonium iodide (NH4I). Superior grade or analytical grade.
6.8 Oxides or salts (depending on the analysis task). Spectrally pure or superior grade.
6.9 Inorganic acid. Analytically grade.
6.10 Plastic ring. Made of polyvinyl chloride material; used to strengthen the powder
briquette sample during the sample preparation process of the powder briquette method.
6.11 Metal ring. Its function is the same as that of plastic ring.
7 Preparation method of sample
7.1 Solid sample preparation method
For bulk samples such as metal, alloy, cast iron, ore, glass, etc., if a suitable standard
sample can be found, the bulk sample can be put into the instrument for measurement,
as long as it is cut and surface polished.
7.2 Powder briquette method
Weigh an appropriate amount of powdery sample, which has a particle size of less than
75 μm.
7.3 Vitreous fusion method
In the gold platinum crucible, quantitatively weigh the analysis sample, the main flux,
the flux aid, the oxidizing agent and the release agent, which has a suitable particle size,
in a certain proportion. After mixing evenly, put the crucible into melting machine or
muffle furnace, which was preheated to 1000 °C ~ 1200 °C for melting. After melting,
transfer to the preheated gold platinum mold, to cool and solidify.
7.4 Solution sample preparation method
Carry out chemical treatment of a solid sample, to convert it into a solution. The
standard solution and the analytical sample solution shall be similar in terms of
composition and pH.
7.5 Thin film sample preparation method
For powder samples, which have a particle size of less than 48 μm, it can be sprayed on
the tape; OR sprayed on the supporting material such as filter paper by spraying
technology; OR the powder sample can be mixed with an organic reagent to form a jelly,
then coated on the supporting material; OR the powder sample is made into a solution,
8 Qualitative analysis
According to the analysis requirements, first determine the measurement conditions (X-
ray tube current and voltage, analyzing crystal, angle scanning range, etc.). Then scan
the specimen. Record the scanning process with a recorder. Then obtain a spectral line
intensity and angle 2θ scanning picture.
9 Semi-quantitative analysis
Select or synthesize a standard sample, which is basically similar to the analytical
sample in terms of chemical composition and physical properties after sample
preparation.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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