CN111239173A - Analysis method for detecting aluminum-zirconium intermediate alloy by X-ray fluorescence spectrometer - Google Patents
Analysis method for detecting aluminum-zirconium intermediate alloy by X-ray fluorescence spectrometer Download PDFInfo
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- CN111239173A CN111239173A CN202010240813.3A CN202010240813A CN111239173A CN 111239173 A CN111239173 A CN 111239173A CN 202010240813 A CN202010240813 A CN 202010240813A CN 111239173 A CN111239173 A CN 111239173A
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 41
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- ZGUQGPFMMTZGBQ-UHFFFAOYSA-N [Al].[Al].[Zr] Chemical compound [Al].[Al].[Zr] ZGUQGPFMMTZGBQ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000004458 analytical method Methods 0.000 title claims abstract description 20
- 238000004876 x-ray fluorescence Methods 0.000 title claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 9
- 238000009614 chemical analysis method Methods 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910000838 Al alloy Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910016952 AlZr Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 abstract description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000005204 segregation Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000012937 correction Methods 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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Abstract
The invention discloses an analysis method for detecting an aluminum-zirconium intermediate alloy by an X-ray fluorescence spectrometer, which establishes an analysis method by collecting and manufacturing a standard sample and determines analysis parameters so as to achieve the aim of detecting the zirconium content (3.00-15.00)% in the aluminum-zirconium intermediate alloy. The method has the advantages that the detection sample is directly an alloy sample block, the detection can be directly carried out only by turning the detection surface, the operation is more convenient, the detection efficiency is improved, the whole detection process does not need to use chemical reagents, the method is more environment-friendly, the detection cost is saved, the detection result is stable and reliable, the influence of component segregation of the alloy ingot is small, and the detection result is more representative.
Description
Technical Field
The invention belongs to the technical field of alloy analysis, and particularly relates to an analysis method for detecting an aluminum-zirconium intermediate alloy by using an X-ray fluorescence spectrometer.
Background
The analysis method of the X-ray fluorescence spectrometer does not have corresponding national standard at present. Currently, there is only a metrological verification procedure in JJG 810 + 1993 wavelength dispersive X-ray fluorescence spectrometer. The component detection method for the aluminum-zirconium intermediate alloy currently comprises the following steps:
① GB/T20975.25-2008 aluminium and aluminium alloy chemical analysis method part 25, inductively coupled plasma atomic emission spectrometry, zirconium element determination range (0.0020-1.00)%.
② GB/T7999 & lt 2015 & gt aluminum and aluminum alloy photoelectric direct reading emission spectrometry, the determination range of zirconium element is (0.0001-0.50)%.
③ GB/T16597 & 1996 analysis method of metallurgy products X-ray fluorescence Spectroscopy general rules, the detection method of the components of the aluminum-zirconium intermediate alloy is not specifically described, and only general matters of quantitative analysis of elements by the X-ray fluorescence Spectroscopy are specified.
In the national standard GB/T/27677-2011 aluminum master alloy, the zirconium element content in the aluminum zirconium master alloy product is higher, and the zirconium element content is mostly required to be (3.00-15.00)%. The measurement ranges of the inductively coupled plasma atomic emission spectrometry and the photoelectric direct-reading emission spectrometry do not cover the detection of the high-content zirconium element. At present, the analysis method for detecting the aluminum zirconium intermediate alloy by using the X-ray fluorescence spectrometer has no corresponding national standard sample.
Disclosure of Invention
The invention aims to provide an analysis method for detecting an aluminum-zirconium intermediate alloy based on an X-ray fluorescence spectrometer. The method establishes an analysis method through collection and preparation of standard samples, and determines analysis parameters so as to achieve the purpose of detecting the zirconium content (3.00-15.00)% in the aluminum zirconium intermediate alloy.
An analysis method for detecting an aluminum-zirconium intermediate alloy by an X-ray fluorescence spectrometer is established by the following specific processes:
(1) collection and preparation of standard samples: adopting national standard samples A356 series, E4121-E4125 and E9021-E9026 as standard samples of metal impurity elements, and preparing standard samples of aluminum-zirconium intermediate alloys AlZr3, AlZr5, AlZr8, AlZr10 and AlZr15 by self;
(2) the self-made aluminum zirconium intermediate alloy standard sample is set as follows: part 25 of the chemical analysis method for aluminum and aluminum alloys by GB/T20975.25-2008: detecting an aluminum zirconium intermediate alloy standard sample by an inductively coupled plasma atomic emission spectrometry;
(3) the method comprises the following steps: the method is established by two detection methods according to the content of main elements of the product: the method comprises the following steps: the main element Zr (3.00-10.00)% standard curve, and the used aluminum zirconium intermediate alloy grades comprise: AlZr3, AlZr5, AlZr8, AlZr 10; the second method comprises the following steps: the main element Zr (10.00-15.00)% standard curve, and the used aluminum zirconium intermediate alloy grades comprise: AlZr10, AlZr 15; the two methods adopt national standard samples A356 series, E4121-E4125 and E9021-E9026 to establish a standard curve of metal impurity elements, which is shown in the figure 1-2;
(4) the method comprises the following steps: the repeatability and correctness verification results of the method meet the standard requirements, and are shown in tables 1-2; the method is adopted to carry out multi-heat and multi-brand comparison by an X-ray fluorescence spectrometer analysis method and an inductively coupled plasma atomic emission spectrometry chemical analysis method. The comparison results meet the standard requirements, see table 3.
TABLE 1 method repeatability validation data
| Number of measurements | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Zr% (sample) | 5.03 | 4.99 | 5.06 | 4.93 | 4.96 | 4.90 | 5.01 | 5.02 | 4.95 | 5.05 |
Table 2 method verification results
TABLE 3 comparison of test results
Further, before the standard sample of the aluminum zirconium intermediate alloy is detected, the standard sample of the aluminum zirconium intermediate alloy needs to be taken and diluted to meet the standard requirement.
Further, the metallic impurity elements in the method establishment include Si, Fe, Cu, Mg, Ca, V, Mn, Ni, Zn, Sn, Ga, Hf.
The analysis method for detecting the aluminum-zirconium intermediate alloy based on the X-ray fluorescence spectrometer has the advantages that:
① fills the blank of the chemical analysis method in the determination range (3.00-15.00)% of zirconium element in the part 25 of the chemical analysis method of GB/T20975.25-2008 aluminum and aluminum alloy, inductively coupled plasma atomic emission spectrometry.
②, the problem that no national standard sample exists in the detection of the aluminum zirconium intermediate alloy by using an X-ray fluorescence spectrometer is solved, the self-made aluminum zirconium intermediate alloy (the brand comprises AlZr3, AlZr5, AlZr8, AlZr10 and AlZr15) standard sample, the zirconium element standard sample used for establishing, monitoring and correcting the standard curve and the drift of the aluminum zirconium intermediate alloy is self-made, the standard curve and the drift correction are carried out by strict test comparison before use, all indexes meet the standard requirements, and the use effect is good.
③ the zirconium content in the aluminum zirconium intermediate alloy is high, so the sample preparation of the inductively coupled plasma atomic emission spectrometry includes not only dissolving, constant volume, but also preparing steps such as dividing, diluting, constant volume, etc., the sample preparation and detection time is long, the method can directly detect the sample which is the alloy sample block, only the detection surface is turned, the operation is more convenient, the detection efficiency is improved, and the method does not need to use chemical reagent in the whole detection process, is more environment-friendly, and saves the detection cost.
④, the detection result is stable and reliable, and is less influenced by the composition segregation of the alloy ingot, and the detection result is more representative.
Drawings
FIG. 1 is a standard curve of (3.00-10.00)% Zr as the main element;
FIG. 2 shows the standard curve of Zr as the main element (10.00-15.00%).
Detailed Description
In order that those skilled in the art can better understand the present invention, the following technical solutions are further described with reference to the accompanying drawings and examples.
An analysis method for detecting an aluminum-zirconium intermediate alloy based on an X-ray fluorescence spectrometer, which comprises the following main elements of Zr content (3.00-15.00)%:
sample preparation: the thickness and the diameter of the sample block should meet the size requirement of the sample cup of the instrument on the sample, a lathe is used for processing the sample into a plane, the turning thickness is 3-5mm, and the sample should be smooth and flat without chips. The detection surface of the sample can not be contacted by hands or other foreign matters, and the detection surface is ensured to be upward when the sample is placed, so that the sample is kept dry and prevented from being polluted.
And (3) sample determination: and checking the state of the instrument, sequentially putting the processed samples into the sample cups, ensuring that the samples completely cover the round holes at the bottoms of the sample cups, ensuring that the thickness of the samples cannot exceed the height of the sample cups, lightly taking the samples to prevent the samples and the sample cups from being damaged, and detecting according to rules.
The method and GB/T20975.25-2008 aluminium and aluminium alloy chemical analysis method part 25: the difference between inductively coupled plasma atomic emission spectrometry lies in that:
① detection range of zirconium content, the detection range of the method is (3.00-15.00)%, and the detection range of GB/T20975.25-2008 is (0.0020-1.00)%.
② the method has the advantages of direct detection of alloy sample by turning the detection surface, convenient operation, high detection efficiency, no need of chemical reagent, environmental friendliness, and low detection cost.
③ the stability of standard curve is confirmed by regular detection of the monitored sample, if the detection result exceeds the range, drift correction is carried out, after drift correction, the monitored sample is detected again to confirm whether the detection result meets the requirement.
The above examples are merely representative of preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (3)
1. An analysis method for detecting an aluminum-zirconium intermediate alloy by an X-ray fluorescence spectrometer is characterized by comprising the following specific steps of:
(1) collection and preparation of standard samples: adopting national standard samples A356 series, E4121-E4125 and E9021-E9026 as standard samples of metal impurity elements, and preparing standard samples of aluminum-zirconium intermediate alloys AlZr3, AlZr5, AlZr8, AlZr10 and AlZr15 by self;
(2) the self-made aluminum zirconium intermediate alloy standard sample is set as follows: part 25 of the chemical analysis method for aluminum and aluminum alloys by GB/T20975.25-2008: detecting an aluminum zirconium intermediate alloy standard sample by an inductively coupled plasma atomic emission spectrometry;
(3) the method comprises the following steps: the method is established by two detection methods according to the content of main elements of the product: the method comprises the following steps: the main element Zr (3.00-10.00)% standard curve, and the used aluminum zirconium intermediate alloy grades comprise: AlZr3, AlZr5, AlZr8, AlZr 10; the second method comprises the following steps: the main element Zr (10.00-15.00)% standard curve, and the used aluminum zirconium intermediate alloy grades comprise: AlZr10, AlZr 15; the two methods adopt national standard samples A356 series, E4121-E4125 and E9021-E9026 to establish a standard curve of metal impurity elements;
(4) the method comprises the following steps: the method is adopted to carry out multi-heat and multi-brand comparison by an X-ray fluorescence spectrometer analysis method and an inductively coupled plasma atomic emission spectrometry chemical analysis method.
2. The analysis method for detecting the aluminum zirconium intermediate alloy by the X-ray fluorescence spectrometer as claimed in claim 1, wherein before the detection of the aluminum zirconium intermediate alloy standard sample, the aluminum zirconium intermediate alloy standard sample needs to be divided and diluted to meet the standard requirement.
3. The method as claimed in claim 1, wherein the metallic impurity elements include Si, Fe, Cu, Mg, Ca, V, Mn, Ni, Zn, Sn, Ga, Hf.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2756666C1 (en) * | 2021-02-01 | 2021-10-04 | Акционерное общество "Чепецкий механический завод" | Method for determining the content of hafnium in metallic zirconium and alloys based on it |
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