CN112945940A - Method for measuring solid powder discharge product of GIS (gas insulated switchgear) by using handheld alloy analyzer - Google Patents
Method for measuring solid powder discharge product of GIS (gas insulated switchgear) by using handheld alloy analyzer Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The invention belongs to the field of analysis and detection, and relates to a method for measuring a solid powder discharge product of GIS equipment by using a handheld alloy analyzer, which comprises the following steps: white paper laying method, plain sheet laying method, metal sheet laying method with grooves and preservative film wrapping method. Different methods are adopted to carry out elemental analysis on the discharge solid powder, and the measurement result deviation of the main elements is not large and is relatively stable. The method has certain guiding significance for the field analysis of the element components of the discharge product of the GIS equipment.
Description
Technical Field
The invention belongs to the field of analysis and test, and particularly relates to a plurality of methods for measuring solid powder discharge products of GIS equipment by using a handheld alloy analyzer.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Gas insulated metal enclosed switchgear, GIS equipment for short, but in the actual operation process, often takes place the accident of discharging. In order to effectively determine the cause of the discharge accident, it is necessary to analyze the discharge product. In the GIS equipment, SF6 gas and a discharge product generated after a metal component is discharged are divided into two types, namely solid powder (sulfide and fluoride) and gas, wherein a chemical analysis method is usually adopted for analyzing the solid powder, but the analysis time is long, so that the requirement on the field analysis of the element components of the discharge product of the GIS equipment is difficult to meet.
Disclosure of Invention
In order to overcome the problems, the invention provides a plurality of methods for measuring solid powder discharge products of GIS equipment by using a handheld alloy analyzer. Different methods are adopted, so that the measurement result deviation of the main elements is not large and is stable. The method has certain guiding significance for the field analysis of the element components of the discharge product of the GIS equipment.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a method for measuring solid powder discharge products of a GIS device by using a handheld alloy analyzer is provided, which comprises the following steps:
collecting solid powder discharge products generated by discharging of GIS equipment as samples;
spreading the sample on white paper, and measuring by using a handheld alloy analyzer;
or, the sample is concentrated in a circular area on the flat elementary metal sheet, and a handheld alloy analyzer is adopted for measurement;
or, the sample is concentrated in a circular groove on the flat elemental metal sheet, and a handheld alloy analyzer is adopted for measurement;
or wrapping the sample with an ultrathin plastic preservative film to enable the measurement window of the handheld alloy analyzer to be vertically upward for measurement;
wherein, the diameters of the circular area and the circular groove are smaller than the diameter of the measuring window; the bottom surface of the wrapped sample should cover the entire measurement window.
In a second aspect of the present invention, there is provided a kit for measuring solid powder discharge products of a GIS device by using a handheld alloy analyzer, comprising: the device comprises a handheld alloy analyzer, white paper, a plastic preservative film, a flat elemental metal sheet or an elemental metal sheet with a groove.
In a third aspect of the invention, the application of the handheld alloy analyzer in the field analysis of the elemental composition of the discharge product of the GIS equipment is provided.
The invention has the beneficial effects that:
(1) the method adopts the white paper bedding method, the flat elementary substance sheet bedding method, the elementary substance metal sheet bedding method with the groove, the preservative film wrapping method and other methods to carry out element analysis on the discharged solid powder, and the measurement results of main elements are not greatly deviated and are relatively stable. If the requirement on the measurement precision is not high or only the main elements are required to be measured more accurately, any one of the three methods can be adopted.
(2) The invention adopts different methods to carry out element analysis on the discharge solid powder, the deviation of the measurement result of the secondary elements is likely to be larger, and at the moment, several methods are adopted as much as possible and are judged according to the actual situation on site or other methods such as a laboratory analysis method are assisted.
(3) In the invention, the flat sheet bedding method is meaningful only when the amount of the discharge solid powder is small (the situation is frequent) and the paving thickness is thin, and the measured data needs to be normalized to obtain the final result.
(4) The test method is simple, convenient to operate, strong in practicability and easy to popularize, and has certain guiding significance for field analysis of the element components of the discharge product of the GIS equipment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a diagram of a handheld alloy analyzer in example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Method for measuring solid powder discharge product of GIS (gas insulated switchgear) by using handheld alloy analyzer
Through a large number of experiments, several feasible methods for measuring the elemental composition of the discharge product by using a handheld alloy analyzer are summarized, and specific operation and applicable conditions of each method and respective advantages and disadvantages are listed, as shown in the following table.
Table 1 several methods for measuring elemental composition of discharge products with a hand-held alloy analyzer
The specific elements of the substrate are not particularly limited in this application, and in some embodiments, the flat metal sheet is a Pb substrate, a Sn substrate, a Si substrate, or a W substrate, so as to select the substrate according to different detection requirements.
In some embodiments, the substrate purity of the flat metal sheet is greater than 99.9%, so that the interference of the substrate on the detection result is reduced, and the detection precision is improved.
In some embodiments, the sample fills the entire circular recess so that the sample is substantially free of interference from the working face composition; avoiding the influence of air turbulence in the surrounding environment.
In some embodiments, the thickness of the sample is greater than 100 microns to reduce the effect of the substrate or background on the detection results and improve detection accuracy.
In some embodiments, the operating temperature is-20 ℃ to +55 ℃ during the measurement, and the operating humidity is: the relative humidity is less than 95 percent, so as to ensure the stability of the testing process and improve the detection precision.
The specific model of the handheld alloy analyzer is not particularly limited in this application, and in some embodiments, the handheld alloy analyzer is provided with an X-ray emitter to perform elemental content measurement using X-rays.
In some embodiments, when the sample thickness is small, the test data is normalized to obtain a final result, and the influence of the substrate on the test result is eliminated through the normalization processing, so that the accuracy of the test result is improved.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
In the following examples, a brook hand-held spectrometer S1TITAN600 was used as the hand-held alloy analyzer. The testing steps comprise: power-on-select sample type-trigger test-output result (can be done with reference to product description).
In the following examples, the purity of each sheet metal substrate was greater than 99.9%.
Example 1:
discharge products of three discharge accidents including a Binzhou 220kV Mingji station, a sunshine 500kV Kyokup station and an east-Ying220 kV Chenzhang station are collected, the numbers of the discharge products are sequentially #1, #2 and #3, the discharge products are subjected to element component analysis after 11 elements, and test results are all listed and are all in percentage by mass.
Sample #1 Binzhou 220kV Mingji station
The test results were as follows:
white paper bedding method: fe: 39.33S: 33.11 Cr: 13.70 Mn: 1.32 Si: < LOD Ni: 0.38 Al: 1.39 Cu: 2.47 As: 0.03 Ti: 0.05 Co: 0.17 Mo: 0.03V: 0.14 Zn: 0.13 Ru: 0.40 Pd: 0.20 Ag: 4.09 In: 0.03 Pt: 0.02 Au: 0.20 Sn: 0.23W: 2.22
A preservative film wrapping method: fe: 43.37S: 22.52 Cr: 14.28 Mn: 1.36 Si: < LOD Pb < LOD Ni: 0.30 Al: 2.42 Cu: 2.27 Ti: 0.11 Co: 0.19 Mo: 0.06V: 0.11 Zn: 0.13 Ru: 0.53 Pd: 0.16 Ag: 8.26 In: 0.80 Pt: 0.05 Au: 0.25 Sn: 0.64W: 2.20
Flat single sheet matting method (Pb substrate method): fe: 34.13S: 16.71 Cr: 10.35 Mn: 0.90 Si: < LOD P: < LOD Ni: 0.25 Al: 2.59 Cu: 2.24 Ti: 0.11 Co: 0.15 Mo: 0.04V: 0.09 Pb: 23.26 Zn: 0.11 Zr: 0.03 Ru: 0.39 Ag: 5.43 In: 0.49 Au: 0.83 Sn: 0.35W: 1.54
The sample is thinner after being spread on the Sn substrate, so that Pb is detected, normalization treatment is required, and the processed data are as follows: fe: 44.47S: 21.77 Cr: 13.49 Mn: 1.17 Si: < LOD P: < LOD Ni: 0.33 Al: 3.38 Cu: 2.92 Ti: 0.14 Co: 0.20 Mo: 0.05V:0.12 Zn: 0.14 Zr: 0.04 Ru: 0.51 Ag: 7.07 In: 0.66 Au: 1.08 Sn: 0.46W: 2.01
Flat single sheet matting method (Si substrate method): fe: 41.99 Si: 25.50 Cr: 13.90 Mn: 1.41 Si: < LOD P: < LOD Ni: 0.33 Al: 2.53 Cu: 2.29 Ti: 0.04 Co: 0.18 Mo: 0.06V: 0.13 Zn: 0.14 Ru: 0.51 Ag: 6.63 In: 1.10 Pt: 0.05 Au: 0.24 Sn: 0.69W: 2.28
And (3) verifying the accuracy:
in the laboratory, the sample was retested using inductively coupled plasma spectroscopy (ICAP), and the results show that: by adopting the method for measuring the solid powder discharge product of the GIS equipment by using the handheld alloy analyzer, the measurement result deviation of the main elements is not large (the contents of the elements in the first three ranks are consistent according to the sorting of the contents), the method is relatively stable, and the requirement of performing preliminary element analysis on the discharge solid powder can be met.
Example 2
The test method was the same as in example 1.
The test results were as follows:
#2 sample sunshine 500kV Kyoho station
White paper bedding method: al: 72.00 Zn: 0.13 Mg: < LOD Ni: 0.27 Ti: 11.30V: 0.43 Mn: 0.51 Fe: 2.01 Zr: 0.31 Ru: 5.16 Rh: 3.33 Pd: 1.56 In: 2.16 Ta: 0.26 Pb: 0.47 Cr: 0.08
A preservative film wrapping method: al: 53.24 Zn: 0.41 Mg: < LOD Ni: 0.40 Ti: 16.38V: 0.78 Mn: 0.91 Fe: 4.10 Co: 0.03 Zr: 0.74 Nb: 0.18 Ru: 8.32 Rh: 7.57 Pd: 1.49 In: 3.75 Re: 0.35 Pb: 1.17 Cr: 0.18
Flat single sheet matting method (Sn substrate method): sn: 88.94 Ag: < LOD Cu: 0.11 Al: 8.03 Mn: 0.12 Fe: 0.19 Co: 0.01 Ni: 0.06 Zn: 0.21 Ta: 0.08 Ti: 1.39V: 0.18 Zr: 0.06 Ru: 0.54Ir 0.05Pb 0.02
Because the sample is thinner after being spread on the Sn substrate, Sn is detected, normalization processing is needed, and the processed data are as follows: al: 72.60 Cu: 0.99 Mn: 1.08 Fe: 1.72 Co: 0.09 Ni: 0.54 Zn: 1.90 Ta: 0.72 Ti: 12.57V: 1.63 Zr: 0.54 Ru: 4.88 Ir: 0.45 Pb: 0.18
The normalization treatment comprises the following specific steps: the end result is the content of each element/(1-content of substrate element), for example: the final Cu content is 0.11%/(1-88.94%) -0.99.
And (3) verifying the accuracy:
in the laboratory, the sample was retested using inductively coupled plasma spectroscopy (ICAP), and the results show that: by adopting the method for measuring the solid powder discharge product of the GIS equipment by using the handheld alloy analyzer, the measurement result deviation of the main elements is not large (the contents of the elements in the first three ranks are consistent according to the sorting of the contents), the method is relatively stable, and the requirement of performing preliminary element analysis on the discharge solid powder can be met.
Example 3
The test method was the same as in example 1.
The test results were as follows:
#3 sample Dongying 220kV Chenzhuang station
White paper bedding method: cu: 94.97 Si: 0.28S: 3.04 Sn: 0.10 Ag: 1.15 Hg: 0.14 Zn: 0.20 Cr: 0.06 Co: 0.02 Zr: 0.03
A preservative film wrapping method: cu: 96.33 Sn: 0.10 Ag: 1.67S: 1.59 Hg: 0.02 Zn: 0.18 Cr: 0.06 Zr: 0.04
Flat single sheet matting method (Pb substrate method): cu: 95.28 Si: 0.21 Sn: 0.08 Ag: 1.59S: 2.35 Ti: 0.05 Zn: 0.21 Hg: 0.10 Cr: 0.05 Pt: 0.02 Co: 0.04 Zr: 0.03
Flat single sheet matting method (W substrate method): cu: 95.02 Si: 0.30 Sn: 0.19S: 2.36 Ag: 1.37 Ti: 0.04 Zn: 0.21 Hg: 0.10 Fe: 0.26
And (3) verifying the accuracy:
in the laboratory, the sample was retested using inductively coupled plasma spectroscopy (ICAP), and the results show that: by adopting the method for measuring the solid powder discharge product of the GIS equipment by using the handheld alloy analyzer, the measurement result deviation of the main elements is not large (the contents of the elements in the first three ranks are consistent according to the sorting of the contents), the method is relatively stable, and the requirement of performing preliminary element analysis on the discharge solid powder can be met.
By comparing and analyzing the above data, the following conclusions can be drawn:
(1) different methods are adopted to carry out elemental analysis on the discharge solid powder, and the measurement result deviation of the main elements is not large and is relatively stable. If the requirement on the measurement precision is not high or only the main elements are required to be measured more accurately, any one of the three methods can be adopted.
(2) When the number of the samples is large and thick, the X-ray cannot penetrate through the samples to be shot onto the testing platform, and the measuring result cannot be interfered. Only when the amount of the discharge solid powder is small and the spread thickness is thin, the method has significance by adopting a flat single sheet bedding method, and the measured data needs to be normalized at the moment to obtain a final result.
The conclusion has certain guiding significance for the field analysis of the discharge product element components of the GIS equipment.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method for measuring solid powder discharge products of GIS equipment by using a handheld alloy analyzer is characterized by comprising the following steps:
collecting solid powder discharge products generated by discharging of GIS equipment as samples;
spreading the sample on white paper, and measuring by using a handheld alloy analyzer;
or, the sample is concentrated in a circular area on one flat metal sheet, and a handheld alloy analyzer is adopted for measurement;
or, the sample is concentrated in a circular groove on the flat metal sheet, and a handheld alloy analyzer is adopted for measurement;
or wrapping the sample with an ultrathin plastic preservative film to enable the measurement window of the handheld alloy analyzer to be vertically upward for measurement;
wherein, the diameters of the circular area and the circular groove are smaller than the diameter of the measuring window; the bottom surface of the wrapped sample should cover the entire measurement window.
2. The method for measuring the GIS device solid powder discharge product by using the handheld alloy analyzer according to claim 1, wherein the flat metal sheet is a Pb substrate, a Sn substrate, a Si substrate or a W substrate.
3. The method for measuring GIS device solid powder discharge products using handheld alloy analyzer as claimed in claim 1 wherein the flat metal sheet has a substrate purity of greater than 99.9%.
4. The method for measuring GIS device solid powder discharge products using handheld alloy analyzer as claimed in claim 1 wherein the sample fills the entire circular groove.
5. The method for measuring GIS device solid powder discharge products using handheld alloy analyzer according to claim 1 wherein the sample thickness is greater than 100 microns.
6. The method for measuring the solid powder discharge product of the GIS equipment by using the handheld alloy analyzer as claimed in claim 1, wherein in the measuring process, the working temperature is-20 ℃ to +55 ℃, and the working humidity is as follows: relative humidity < 95%.
7. The method for measuring GIS device solid powder discharge products using handheld alloy analyzer according to claim 1, wherein the handheld alloy analyzer is provided with an X-ray emitter.
8. The method for measuring the GIS device solid powder discharge product by using the handheld alloy analyzer as claimed in claim 1, wherein when the sample thickness is thin, the test data is normalized to obtain the final result.
9. A kit for measuring solid powder discharge products of GIS equipment by using a handheld alloy analyzer is characterized by comprising: a hand-held alloy analyzer, white paper, plastic preservative film, flat metal sheet, or flat metal sheet with grooves.
10. The application of the handheld alloy analyzer in the field analysis of the discharge product element components of the GIS equipment.
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