CN114113291A - Method for determining content of main element in multi-element alloy by using proportional coefficient correction glow mass spectrometry - Google Patents
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Abstract
The invention relates to a method for determining the content of a main element in a multi-element alloy by a proportional coefficient modification glow mass spectrometry, belonging to the technical field of analysis and test. A glow discharge mass spectrometer is adopted to measure a group of multi-element alloys with different main elements and different contents, and the mass count of the main elements is obtained; establishing a quantitative ratio coefficient of the content of the main quantity element to the massf(ii) a Finally, the mass count of the main element in the multi-element alloy sample to be detected is rapidly obtained by utilizing glow discharge mass spectrometry, and the mass count is calculated according to the proportionality coefficientfAnd (5) correcting and quantitatively obtaining the content of the main element. The method uses the constant-value multi-component alloy to establish the mass counting proportion coefficient relation with the glow discharge mass spectrometry so as to quantitatively determine the content of the main component element in the multi-component alloy, has the advantages of rapidness, accuracy, reliability and the like, and is an effective content analysis method for the main component element in binary and ternary alloy materials.
Description
Technical Field
The invention relates to a method for determining the content of a main element in a multi-element alloy by a proportional coefficient modification glow mass spectrometry, belonging to the technical field of analysis and test.
Background
The multi-element alloy of titanium, nickel, cobalt, iron, etc. is widely applied to the fields of military affairs, aerospace, etc. and the advanced national defense industry and civil industry, for example, the intermediate alloy of Ni-Cr alloy, Ni-Mg alloy, Al-V alloy, Ni-B alloy, Ni-Ca alloy, Fe-Cr-Al alloy, Ni-Cr-Mo alloy, Fe-Cr-Ni-Mo alloy, etc. is an important raw material for producing titanium, nickel, cobalt and iron alloy, and can mainly improve the heat resistance and cold processing performance of the alloy, so that the alloy has good welding performance and quite high mechanical strength. The multi-component alloy generally consists of metal elements or metal elements and nonmetal elements and has a metallic characteristic. Most alloys often contain multiple elements due to production and actual material purity. From the organizational structure, the multi-element alloy is relatively complex, and the research on the interaction mechanism between the finished product of each component and each element has strong guiding significance for the practical application of the multi-element alloy.
The determination of the main element in the multi-element alloy, especially binary and ternary alloy, is generally weight method, chemical titration method, inductively coupled plasma atomic emission spectrometry, etc. Chinese patent No. CN106841154B discloses a method for determining the content of calcium in nickel-calcium alloy by fluorescence titration; CN103760051B discloses a method for measuring silicon in a silicon-zirconium alloy by a gravimetric method and zirconium by a titration method; CN 103529165A discloses an EDTA titration method for directly determining the aluminum content in a vanadium-aluminum alloy; lanna Pinna et al used EDTA titration to determine nickel and magnesium in nickel-magnesium alloys; the Nissan Junqiang et al use inductively coupled plasma atomic emission spectrometry to determine zirconium in silicon-zirconium alloy. In the detection method of CSM 04180501 and 2001 nickel-boron alloy-determination of boron content-neutralization titration method, sodium hydroxide standard solution is used for titrating boric acid.
The gravimetric method in the detection method has various steps and overlong determination time; the titration method generally adopts a complex titration method, the reaction rate is slow at normal temperature, the titration interference is serious, the end point can repeatedly appear, and the observation is difficult; the inductively coupled plasma atomic emission spectrometry is mainly used for micro-measurement, and a large amount of acid and alkali is required to be added for sample dissolution, so that a large amount of reagents are consumed, and the environment is polluted. Glow Discharge Mass Spectrometry (GDMS) is used as a solid sample direct analysis technology, when a sample is measured, Relative Sensitivity Factor (RSF) data is needed to be used for converting ion current intensity, and a relation between the content of each element and the ion current intensity is established, for example, research on relative sensitivity factors in glow discharge mass spectrometry of Tang Yichuan and the like, the method is widely applied to analysis of trace and ultra-trace impurity content of materials such as high-purity metals, semiconductors and the like, but because the method is influenced by factors such as mass spectrum interference and the like, for example, various interference types listed in Multi-element glow discharge mass spectrometry determination and interference correction of high-temperature alloys of Yunxing paper and the like, the direct quantitative analysis of the content of the main element in the sample has certain difficulty. Therefore, Glow Discharge Mass Spectrometry (GDMS) has been applied to qualitative semi-quantitative analysis of trace, and ultra-trace elements, limiting its application to analysis of major element content in multi-component samples.
Disclosure of Invention
The invention aims to overcome the defects in the existing glow discharge mass spectrometry technology and provide a method for determining the content of a main element in a multi-element alloy by using a proportional coefficient correction glow mass spectrometry.
The technical scheme of the invention is a method for determining the content of a main element in a multi-element alloy by a proportional coefficient modification glow mass spectrometry, which comprises the following steps:
(1) determining accurate content C of a group of known main quantity elements by adopting glow discharge mass spectrometeriIn the multi-component alloy of (2), the mass count C of the major elements is obtainedRi；
(2) The content C of the principal component element is established by adopting a linear regression methodiCount the mass CRiCoefficient of proportionality fi；
(3) Rapidly obtaining mass count C of main elements in multi-element alloy sample to be detected by glow discharge mass spectrometryRxBy a coefficient of proportionality fiCorrecting and quantitatively obtaining the content C of the main elementx。
Preferably, the accurate content C of the major element in the step (1)iThe quantitative test method comprises one or more of chemical titration method, gravimetric method and spectral method.
Preferably, the multi-component alloy in the step (1) is a binary or ternary alloy.
Preferably, the binary or ternary alloy in step (1) is specifically a Ni-Cr alloy, a Ni-Mg alloy, an Al-V alloy, a Ni-B alloy, a Ni-Ca alloy, a Fe-Cr-Al alloy or a Ni-Cr-Mo alloy.
Preferably, the multicomponent alloy obtained in step (1) is prepared, and can be a standard substance with known main element content or a block sample with the diameter larger than 10mm prepared by the same type of the setting value obtained in step (3).
Preferably, the surface of the multi-element alloy sample prepared in the step (1) is uniform, the excitation signal is stable when the multi-element alloy sample is tested by a glow discharge mass spectrometer, and the relative standard deviation of 3 continuous mass counts is less than 0.5%.
Preferably, the proportionality coefficient f in step (2)i＝(CRi±bi)/Ci(ii) a Wherein b isiIs a mass count correction value.
Preferably, at least 3 samples are used in step (2) using linear regression.
Preferably, the content C of the main element in the sample to be detected in the step (3)x＝(CRx±bi)/fi。
The invention abandons the relatively mature and complex calculation process of glow mass spectrometry relative sensitivity factor method (RSF) theory principle, in the test mechanism, the element quantitative determination is carried out by utilizing the measurement relation established by the counting signal intensity generated after the excitation of the fixed charge-mass ratio corresponding to each element in the mass spectrometry and the content of the element to be detected in the analyte, and because the measurement relation is influenced by the factors such as environment, the matching degree of the calibration substance matrix, the mass spectrometry interference and the like, the deviation is generated, so the mass counting correction is needed; the invention can be used for accurately measuring trace elements and can also be used for accurately measuring main elements. Because the functional characteristics of glow mass spectrometer are mainly in the detection of trace or trace elements, and the number of trace or trace elements with accurate definite value in the solid alloy standard sample is less, one portion of multi-element alloy standard sample used in said invention contains main element content, and even if the alloy standard sample has no or less quantity, it can use traditional chemical method to make accurate definite value, and then the alloy standard sample can be used for making accurate definite valueThen used for establishing a calibration curve by glow mass spectrometry to obtain a proportionality coefficient fiAnd a correction value biSo that the method can be directly applied to quantitative determination of main elements in the multi-element alloy.
The invention has the beneficial effects that: the invention fully embodies the advantages of instrumental analysis, such as higher detection speed than the traditional chemical method, stable and accurate detection result and no pollution.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The following examples used a glow discharge mass spectrometer (Thermo Fisher, usa) of type Element-GD with a discharge current of 35.0mA as the operating parameter; the discharge voltage is 1000V; the flow rate of glow gas is 350 mL/min; the high resolution control pressure is 0.50 MPa; the external voltage is-1600V; the focusing voltage is-800V; the focusing voltage in the X direction is 3.5V; the Y-direction focusing voltage is 1.3V; the shaping voltage is 100V; the filter lens voltage is 4.5V.
Example 1 is described taking a Ni — Cr alloy as an example:
a. determination of Cr in Ni-Cr alloys, reference standard HB 5220.15-2008: putting 5 Ni-Cr chip-shaped samples-1-5 with different Ni and Cr contents into a 500mL conical flask, adding hydrochloric acid and nitric acid, heating to dissolve, and adding sulfuric acid-phosphoric acid mixed acid. Adding nitric acid dropwise for oxidation, adding water, adding silver nitrate and ammonium persulfate solution, and heating for oxidation to purple. Adding sodium chloride for reduction. Using N-phenylated o-aminobenzoic acid as an indicator, titrating by using a ferrous ammonium sulfate standard solution to obtain the mass fraction C of each sampleCriThe results are shown in Table 1.
b. Determination of Ni in Ni-Cr alloys, reference standard HB 5220.23-2008: putting 5 Ni-Cr chip-shaped samples-1-5 with different Ni and Cr contents in a beaker, adding hydrochloric acid and nitric acid, heating and dissolving, precipitating nickel by dimethylglyoxime in an ammonium medium containing citrate, analyzing the precipitate and filter paper by nitric acid and perchloric acid, titrating nickel by EDTA (ethylene diamine tetraacetic acid) standard solution by using ammonium pruurate as an indicator under the condition that the pH value of a test solution is 10 to obtain the mass fraction C of each sampleNiiThe results are shown in Table 1.
c. Taking the 5 Ni-Cr samples-1-5, preparing the samples into block samples meeting the analysis of a glow mass spectrometer, and testing the block samples under the condition of uniform instrument parameters to obtain the mass count C of each element in each sampleRCrAnd CRNiThe results are shown in Table 1.
d. The content C of the main element is established by adopting a linear regression methodiCount the mass CRiCalculating to obtain a proportionality coefficient fiAnd a mass count correction value biThe results are shown in Table 1;
e. rapidly measuring Cr element and Ni element in Ni-Cr alloy sample by glow discharge mass spectrometer to obtain mass count CRxBy a coefficient of proportionality fiCorrecting and quantitatively obtaining the content C of the main elementxThe results are shown in Table 2.
TABLE 1 proportionality factor fiEstablishing
TABLE 2 test results
Example 2 illustrates a ternary Mg-Al-V alloy:
a. and (3) determining Mg in the Mg-Al-V ternary alloy according to the reference standard GB/T20975.16-2008: putting a Mg-Al-V ternary alloy crumb-shaped sample into a 500mL beaker, heating and dissolving the sample by hydrochloric acid, adding nitric acid to complete dissolution, and filtering residues; after ashing, adding sulfuric acid, hydrofluoric acid and nitric acid for dissolving, emitting sulfuric acid smoke, adding hydrochloric acid for dissolving, adding hydrogen peroxide, potassium cyanide and a small amount of iron, separating magnesium from a large amount of aluminum by using NaOH to precipitate magnesium, separating iron, manganese, aluminum and the like again, titrating magnesium by using a CyDTA standard solution by using methyl thymol blue as an indicator, and calculating the mass fraction C of magnesiumMgiThe results are shown in Table 3.
b. Determination of Al in a Mg-Al-V ternary alloy, with reference to the standard YS/T1075.8-2015: dissolving Mg-Al-V ternary alloy scrap-shaped samples 1-5 in a platinum crucible by using hydrofluoric acid and nitric acid, drying, then melting by using lithium tetraborate, a lithium bromide flux and an oxidant, casting into a glass fuse piece, measuring by using an X-fluorescence spectrometer under the selected instrument test condition, and calculating the mass fraction C of aluminum according to a calibration curveAliThe results are shown in Table 3.
c. Determination of V in a Mg-Al-V ternary alloy, reference standard YS/T1075.4-2015: putting 1-5 Mg-Al-V ternary alloy scrap-shaped samples into a 500mL conical flask, adding sulfuric acid-phosphoric acid-nitric acid, heating and dissolving at low temperature, then exhausting sulfuric acid smoke at high temperature, oxidizing vanadium IV to vanadium V by potassium permanganate at room temperature, analyzing excessive potassium permanganate by sodium nitrite in the presence of urea, taking N-phenylated o-aminobenzoic acid potassium as an indicator, titrating by ammonium ferrous sulfate standard solution until mauve turns into bright green, and calculating the mass fraction C of vanadiumViThe results are shown in Table 3.
d. Taking 5 Mg-Al-V ternary alloy samples 1-5, preparing the samples into block samples meeting the analysis of a glow mass spectrometer, and testing the block samples by using the glow mass spectrometer under the condition of uniform instrument parameters to obtain the mass count C of each element in each sampleRiThe results are shown in Table 3.
e. The content C of the main element is established by adopting a linear regression methodiCount the mass CRiCalculating to obtain a proportionality coefficient fiAnd a mass count correction value biThe results are shown in Table 3.
f. Rapidly measuring Mg element, Al element and V element in 2 Mg-Al-V ternary alloy samples by using glow discharge mass spectrometer to obtain mass count CRxBy a coefficient of proportionality fiCorrecting and quantitatively obtaining the content C of the main elementxThe results are shown in Table 4.
TABLE 3 proportionality factor fiEstablishing
TABLE 4 test results
The data results in tables 1 and 3 show that the content of the main element in the multi-element alloy has good linear relation with the mass counting measured by glow discharge mass spectrometry, and R is2>0.9995; the data results in tables 2 and 4 show that the results of the main quantity elements in the multi-element alloy tested by glow discharge mass spectrometry and corrected by the proportionality coefficient are basically consistent with the results of the traditional chemical or spectral method and even superior to the results of the fluorescence spectroscopy. The method meets the requirements of production detection and is beneficial to popularization and application of the detection technology in production.
The above-mentioned examples only express the specific embodiments of the present invention, but should not be construed as limiting the scope of the present invention. Any modifications of the present invention which would occur to those skilled in the art and which are within the spirit of the invention are considered to be within the scope of the present invention.
Claims (9)
1. A method for determining the content of a main element in a multi-element alloy by using a proportional coefficient modification glow mass spectrometry is characterized by comprising the following steps:
(1) determining accurate content of a group of known main quantity elements by adopting glow discharge mass spectrometerC i In the multi-component alloy of (2), obtaining a mass count of the principal component elementC Ri ；
(2) The content of the main quantity element is established by adopting a linear regression methodC i Count the massC Ri Coefficient of proportionality off i ；
(3) Rapidly obtaining mass count of main element in multi-element alloy sample to be detected by glow discharge mass spectrometryC Rx In a proportional coefficientf i Correcting and quantitatively obtaining the content of the main elementC x 。
2. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: the accurate content of the main quantity elements in the step (1)C i The quantitative test method comprises one or more of chemical titration method, gravimetric method and spectral method.
3. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: the multi-element alloy in the step (1) is binary or ternary alloy.
4. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 3, wherein: the binary or ternary alloy is specifically a Ni-Cr alloy, a Ni-Mg alloy, an Al-V alloy, a Ni-B alloy, a Ni-Ca alloy, a Fe-Cr-Al alloy or a Ni-Cr-Mo alloy.
5. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: the multi-element alloy in the step (1) is obtained by preparation, and can be a standard substance with known main element content, or a block sample with the diameter larger than 10mm is prepared by the same type of the setting value in the step (3).
6. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: the multi-element alloy sample prepared in the step (1) has a uniform surface, and when a glow discharge mass spectrometer is used for testing, an excitation signal is stable, and the relative standard deviation of continuous 3-time mass counting is less than 0.5%.
7. The scalefactor modified glow mass spectrometry assay multiplex of claim 1The method for determining the content of major elements in gold is characterized by comprising the following steps: the proportionality coefficient in the step (2)f i =（C Ri ±b i ）/C i (ii) a Whereinb iIs a mass count correction value.
8. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: and (3) at least adopting a linear regression method in the step (2).
9. The method for determining the content of the main element in the multi-element alloy by the proportional coefficient modification glow mass spectrometry as claimed in claim 1, wherein: the content of the main element in the sample to be detected in the step (3)C x =（C Rx ±b i ）/f i 。
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