CN113324979A - Quantitative analysis and determination method of aluminum-niobium alloy - Google Patents
Quantitative analysis and determination method of aluminum-niobium alloy Download PDFInfo
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Abstract
The invention relates to a quantitative analysis and determination method of an aluminum-niobium alloy, which comprises the following steps: preparing a sample solution to be tested: preparing an aluminum-niobium alloy sample into a sample solution to be detected; wherein the to-be-detected sample solution also contains a copper internal standard element; preparing a working curve series solution: preparing a working curve series solution with gradient concentration of the element to be detected; the element to be detected is one or two of aluminum element and niobium element; wherein the working curve series solution also contains a copper internal standard element; detection and analysis steps: and measuring and analyzing the working curve series solution and the sample solution to be measured by using an inductively coupled plasma spectrometer, and calculating the content of the element to be measured in the aluminum-niobium alloy sample. The method is mainly used for providing the quantitative analysis and determination method of the aluminum-niobium alloy, which is simple, convenient, rapid, accurate and reliable to operate, so that the requirements of production enterprises and downstream customers on accurate detection of large-batch aluminum-niobium alloys are met.
Description
Technical Field
The invention relates to the technical field of analytical chemistry and physicochemical inspection, in particular to a quantitative analysis and determination method of an aluminum-niobium alloy.
Background
The master alloy is an important material, is closely related to the life of people and has wide application. With the development of three important industries of aerospace, construction and automobile, the demand for aluminum intermediate alloy is continuously increased, and particularly the consumption of manufacturing industries such as airplanes, trains, ships and the like is continuously increased; the scale and production of aluminium master alloys has developed dramatically in recent years.
The Al-Nb master alloy is an important master alloy for producing high-performance titanium alloy, and has the functions of improving alloying conditions, improving the uniformity of alloy components, overcoming segregation and infusible (refractory) metal inclusion and reducing the metal burning loss rate. With the development of high-end titanium alloys for aerospace use, more severe requirements are put forward on the fluctuation range of main elements of vanadium-aluminum, molybdenum-aluminum and aluminum-niobium intermediate alloys. Aluminum and niobium are main component elements of the aluminum-niobium intermediate alloy and are important control indexes influencing the product quality. The content of aluminum and niobium is the key of the quality of the intermediate alloy product, and plays a very key role in promoting the large-scale and simple production of the titanium alloy.
For the analysis of the macroelements in the metal material, the common methods are inductively coupled plasma spectroscopy (ICP), X-ray fluorescence spectroscopy (XRF), classical volumetric method and gravimetric method.
The national standard GB/T20975.37-2020 aluminium and aluminium alloy chemical analysis method does not list the determination of aluminium element therein, and can not meet the requirements of aluminium intermediate alloy production, application and domestic and foreign trade for large-scale rapid detection at present.
The detection of high content of niobium element (mass fraction 15-90%) is generally carried out by chromatography gravimetric method on paper. In chemical analysis, it is generally accepted that: the precision and accuracy of classical gravimetric and volumetric methods are superior to modern instrumental methods. The classical gravimetric method and volumetric method have the advantages of high analysis accuracy, simple device, good separation effect, mild separation conditions and the like, but have the defects of complex operation and long time consumption.
Inductively coupled plasma atomic emission spectrometry (ICP-AES) is an instrument analysis method which is rapidly developed in recent years, has the advantages of high analysis speed, simple sample introduction, high resolution, small spectral line interference, capability of simultaneously measuring multiple elements, low maintenance and operation cost and the like, is an advanced technical means for analyzing the components of the current constant and trace elements, and has the upper limit of 20 percent of the detection generally. The greatest difficulty of ICP-AES detection is as follows: the detection of elements with high content has the problems of poor data stability and large deviation.
In summary, no industry standard or national standard for simultaneously detecting high content of niobium and aluminum in the aluminum-niobium master alloy has been established so far. Therefore, a method for analyzing niobium and aluminum elements in an aluminum-niobium alloy, which is simple and rapid to operate and has accurate and reliable analysis results, is urgently needed to perfect the technical inadaptable current situation of GB/T20975-.
Disclosure of Invention
In view of this, the present invention provides a quantitative analysis and determination method for an aluminum-niobium alloy, which mainly aims to rapidly, accurately and reliably analyze the contents of niobium and aluminum in the aluminum-niobium alloy, and is simple and convenient to operate.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides a method for quantitative analysis and determination of an aluminum-niobium alloy, which includes the following steps:
preparing a sample solution to be tested: preparing an aluminum-niobium alloy sample into a sample solution to be detected; wherein the to-be-detected sample solution also contains a copper internal standard element;
preparing a working curve series solution: preparing a working curve series solution with gradient concentration of the element to be detected; the element to be detected is one or two of aluminum element and niobium element; wherein the working curve series solution also contains a copper internal standard element;
detection and analysis steps: and measuring and analyzing the working curve series solution and the sample solution to be measured by using an inductively coupled plasma spectrometer, and calculating the content of the element to be measured in the aluminum-niobium alloy sample.
Preferably, the step of preparing a sample solution to be tested includes: mixing an aluminum-niobium alloy sample, water and mixed acid, and heating at a set temperature to completely dissolve the aluminum-niobium alloy sample to obtain a sample solution; adding a copper internal standard solution into the sample solution, and fixing the volume to a set volume to obtain a sample solution to be measured; preferably, after the copper internal standard solution is added into the sample solution, water is added into the sample solution to be constant to a set volume.
In the sample solution: the mass of the aluminum-niobium alloy sample is 0.10 +/-0.0001 g, and the volume of the water is 8-20 mL; the volume of the mixed acid is more than or equal to 15mL, preferably less than or equal to 25 mL; preferably, the water is deionized water; preferably, the mixed acid is mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid; further preferably, in the mixed acid: the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is (0.5-1.5): (0.5-1.5): (0.5-1.5), preferably 1: 1; preferably, the set temperature is 60-80 ℃ and the heating time is 90 minutes or more.
Preferably, after the copper internal standard solution is added into the sample solution, water is added into the sample solution to be constant to a set volume.
Preferably, the copper internal standard solution is determined according to the intensity ratio of the element to be detected and the copper internal standard element corresponding to the inductively coupled plasma spectrometer (here, the copper internal standard solution corresponding to the intensity value close to the element to be detected is added according to the intensity ratio of the element to be detected and the internal standard element corresponding to the instrument, the internal standard content can be flexibly added due to different intensity ratios of different instruments); preferably, if the inductively coupled plasma emission spectrometer is an Aglient5800 type inductively coupled plasma emission spectrometer, the amount of the copper internal standard solution is such that the content of the copper internal standard element in the sample solution to be detected is 30mg ± 0.1 mg.
Preferably, in the step of preparing the working curve series solution: the working curve series solution comprises a plurality of working curve solutions, and the concentration of the element to be detected in the working curve solutions is sequentially increased; wherein the concentration of each element to be detected in the solution of the first working curve is 0.03-0.05mg/mL, preferably 0.04 mg/mL; preferably, the difference value of each element to be detected concentration of the solution of the latter working curve and the solution of the former working curve is 0.015-0.025mg/mL, and preferably 0.02 mg/mL; preferably, the series of working curve solutions comprises 6 working curve solutions.
Preferably, the mass of the copper internal standard element in each working curve solution is the same as the mass of the copper internal standard element in the sample solution to be detected.
Preferably, each working curve solution is prepared from a standard solution of an element to be detected, a standard solution of a copper internal standard, mixed acid and water; the volume of the working curve solution is consistent with that of the sample solution to be detected; the volume of the mixed acid in the working curve solution is the same as that of the mixed acid in the sample solution to be detected; the volume of the copper internal standard solution in the working curve solution is the same as that of the copper internal standard solution in the sample solution to be detected; the standard solution of the element to be detected comprises one or two of an aluminum standard solution and a niobium standard solution; preferably, the preparation steps of each working curve solution are as follows: and mixing the element standard solution to be measured, the copper internal standard solution and the mixed acid, and then adding water into the mixture to fix the volume to a set volume.
Preferably, in the detecting and analyzing step:
detecting the working curve series solution by using an inductively coupled plasma spectrometer, measuring the intensity of the element to be measured and the copper internal standard element, and drawing a working curve by using the mass concentration of the element to be measured as a horizontal coordinate and the intensity ratio of the element to be measured and the internal standard element as a vertical coordinate;
and detecting the sample solution to be detected by adopting an inductively coupled plasma spectrometer, determining the strength ratio of the element to be detected and the internal standard element in the aluminum-niobium alloy sample, calculating the mass concentration of the element to be detected in the sample solution to be detected through the working curve, and further calculating the mass fraction of the element to be detected in the aluminum-niobium alloy sample.
Preferably, the mass fraction of the element to be measured in the aluminum-niobium alloy sample is calculated according to the following formula:
wherein rho is the mass concentration of an element to be detected in a sample solution to be detected, and the unit is mu g/mL;
v is the total volume of the sample solution to be detected, and the unit is mL;
m0the mass of the aluminum-niobium alloy sample is given in g.
Preferably, in the detecting and analyzing step:
if the element to be detected is niobium, taking Nb319.4nm as a spectral line to be detected and Cu327.3nm as an internal standard spectral line;
and if the element to be detected is aluminum, taking Al394.4nm, Al396.1nm as a spectral line to be detected and Cu327.3nm as an internal standard spectral line.
Compared with the prior art, the quantitative analysis and determination method of the aluminum-niobium alloy at least has the following beneficial effects:
the quantitative analysis and determination method for the aluminum-niobium alloy provided by the invention adopts inductively coupled plasma atomic emission spectrometry (ICP-AES) combined with an internal standard method (copper internal standard is selected) to perform quantitative analysis and determination on the aluminum-niobium alloy, realizes rapid, accurate and reliable analysis of the contents of niobium and aluminum in the aluminum-niobium alloy, and is simple and convenient to operate. Meanwhile, the quantitative analysis and determination method for the aluminum-niobium alloy provided by the invention is also an analysis method which is superior to a gravimetric method in the repeatability and accuracy of the analytical test indexes of the spectroscopy analysis which is few in the history of the analytical chemical operation.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a graph showing the relationship between the amount of hydrofluoric acid used and the emission intensity of niobium;
FIG. 2 is a graph showing the relationship between the amount of mixed acid (hydrochloric acid and nitric acid in a volume ratio of 1: 1) and the emission intensity of aluminum element;
FIG. 3 is a graph showing the relationship between the sample dissolution time and the emission intensity of Al and Nb elements in an Al-Nb alloy sample when a sample solution is prepared.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The contents of aluminum and niobium in the aluminum-niobium alloy are high, and the greatest difficulty of ICP-AES detection is that when elements with high contents are detected, the problems of poor data stability and large deviation exist. In order to apply the ICP-AES method to the sample analysis of the aluminum-niobium alloy, the invention firstly proposes the following conception: the ICP-AES and the internal standard method are combined together, and accurate determination of high-content niobium and aluminum elements is realized. The internal standard method is characterized in that a proper internal standard is selected to effectively compensate the matrix effect, the internal standard method is widely applied to analysis of constant, trace and ultra-trace components, and short-term and long-term drift of an analysis signal is monitored and corrected simultaneously, so that the upper limit of detection and the accuracy of an analysis result are improved.
However, the inventor of the present invention has found that while proposing the above concept, there is a technical problem that: and (4) selecting an internal standard. If the conventional internal standard yttrium element is selected, yttrium can form precipitates in a hydrofluoric acid medium and cannot coexist, and the hydrofluoric acid can dissolve niobium element (the niobium element is unstable and is easy to separate out if the hydrofluoric acid is not added into the mixed acid). Further, when another internal standard element is selected (for example, an iron internal standard element), there is a problem that the stability of the measurement result is poor.
Based on the above problems, the inventors of the present invention have made extensive studies to propose: the ICP-AES method for detecting the aluminum-niobium alloy selects the copper internal standard element, can accurately measure high-content niobium and aluminum elements, and has high precision and excellent stability.
The scheme of the invention is as follows:
preparing a sample solution to be tested: preparing an aluminum-niobium alloy sample into a sample solution to be detected; wherein, the sample solution to be detected also contains copper internal standard element.
The method comprises the following steps: mixing an aluminum-niobium alloy sample, deionized water and hydrochloric acid-nitric acid-hydrofluoric acid mixed acid, heating at a constant temperature, and cooling to obtain a sample solution after the sample is completely dissolved; and then adding a copper standard solution into the sample solution, and fixing the volume to a set volume to obtain a sample solution to be detected.
Preferably, the specific operation process of the above steps is as follows: weighing 0.10g (accurate to 0.0001g) of aluminum-niobium alloy sample in a 150mL polyethylene beaker, adding 8-20mL of deionized water and a proper amount of hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (the volume ratio of hydrochloric acid to nitric acid to hydrofluoric acid is 1: 1; the volume of the mixed acid is more than or equal to 15mL, preferably less than or equal to 25mL), placing the mixture on a constant-temperature electric heating plate for constant-temperature heating (the heating time is at least 90 minutes), completely dissolving the sample to obtain a sample solution, cooling, transferring the sample solution into a 250mL polyethylene volumetric flask, adding a copper internal standard solution into the sample solution, and performing constant volume shaking (constant volume with deionized water) to obtain a sample solution to be detected.
Preparing a working curve series solution: preparing a working curve series solution with gradient concentration of the element to be detected; the element to be detected is one or two of aluminum element and niobium element (only one of the elements can be detected, or two elements can be detected simultaneously; if two elements are detected simultaneously, the concentration of the element to be detected refers to the concentration of each element to be detected); wherein, the working curve series solution also contains copper internal standard element.
The method comprises the following steps: the working curve series solution comprises a plurality of working curve solutions, and the concentration of the element to be detected in the working curve solutions is sequentially increased; wherein the concentration of each element to be detected in the solution of the first working curve is 0.03-0.05mg/mL, preferably 0.04 mg/mL; preferably, the difference value of each element to be detected concentration of the solution of the latter working curve and the solution of the former working curve is 0.015-0.025mg/mL, and preferably 0.02 mg/mL; preferably, the series of working curve solutions comprises 6 working curve solutions.
Preferably, the configuration of each working curve solution is as follows: and mixing the element standard solution to be measured, the copper internal standard solution and the hydrochloric acid-nitric acid-hydrofluoric acid mixed acid, and adding water to the mixture to fix the volume to a set volume to obtain a working curve solution. The adding volume of the copper internal standard solution and the adding volume of the mixed acid are consistent with the using amounts of the copper internal standard solution and the mixed acid in the sample solution to be detected; the dosage of the standard solution of the element to be detected depends on the concentration of the element to be detected in the prepared corresponding working curve solution.
If the element to be measured is aluminum and niobium (i.e. the contents of aluminum and niobium in the aluminum-niobium alloy are measured simultaneously), the preferable preparation steps of the working curve series solution are as follows: respectively taking 10mL, 15mL, 20mL, 25mL, 30mL and 35mL of 1000 mu g/mL Al standard solution, sequentially adding the Al standard solution into a No. 1-6 250mL volumetric flask, and taking 10mL, 15mL, 20mL, 25mL, 30mL and 35mL of 1000 mu g/mL Nb standard solution, sequentially adding the Nb standard solution into a No. 1-6 250mL volumetric flask; then, respectively adding a copper internal standard solution (the volume of which is consistent with that of the copper internal standard solution added when the sample solution to be detected is prepared) and a hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (the volume of which is consistent with that of the mixed acid added when the sample solution to be detected is prepared) into No. 1-6 volumetric flasks, diluting with water to constant volume scales, and uniformly mixing to obtain a working curve series solution; wherein, the mass concentrations of Al and Nb are 0.04mg/mL, 0.06mg/mL, 0.08mg/mL, 0.10mg/mL, 0.12mg/mL and 0.14mg/mL in sequence.
Detection and analysis steps: and measuring and analyzing the working curve series solution and the sample solution to be measured by using an inductively coupled plasma spectrometer, and calculating the content of the element to be measured in the aluminum-niobium alloy sample. In addition, in the detection and analysis step, Nb319.4nm is taken as a spectral line to be detected, and Cu327.3nm is taken as an internal standard spectral line; and detecting by using Al394.4nm, Al396.1nm as spectral lines to be detected and Cu327.3nm as internal standard spectral lines.
The method comprises the following steps: detecting the working curve series solution by using an inductively coupled plasma spectrometer, measuring the intensity of the element to be measured and the copper internal standard element, and drawing a working curve by using the mass concentration of the element to be measured as a horizontal coordinate and the intensity ratio of the element to be measured and the internal standard element as a vertical coordinate; and detecting the sample solution to be detected by adopting an inductively coupled plasma spectrometer, determining the strength ratio of the element to be detected and the internal standard element in the aluminum-niobium alloy sample, calculating the mass concentration of the element to be detected in the sample solution to be detected through the working curve, and further calculating the mass fraction of the element to be detected in the aluminum-niobium alloy sample.
The mass fraction of the elements to be detected in the aluminum-niobium alloy sample is calculated according to the following formula:
wherein rho is the mass concentration of an element to be detected in a sample solution to be detected, and the unit is mu g/mL;
v is the total volume of the sample solution to be detected, and the unit is mL;
m0the mass of the aluminum-niobium alloy sample is given in g.
The quantitative analysis and determination method for the aluminum-niobium alloy can be used for simultaneously and rapidly analyzing the main component elements. The method of the invention fully refers to the production technology level of the vanadium-aluminum and molybdenum-aluminum intermediate alloy production enterprises and the use and processing enterprises in China. The method is finally formed by providing innovative design according to actual requirements and carrying out a large number of related experiments. The method is simple and rapid to operate, has accurate and reliable analysis results, is beneficial to the production to carry out product quality inspection work by adopting a uniform analysis method, is beneficial to the formation of a market fair trading environment, and has great social benefits. Meanwhile, the method of the invention also analyzes the repeatability and accuracy of the spectral analysis test index which is rarely used in the history of chemical operation and is better than that of the gravimetric method.
The invention is further illustrated in detail below by means of specific examples:
the aluminum-niobium alloy sample is usually dissolved by adopting a mixed acid of hydrochloric acid, hydrofluoric acid and nitric acid, in a mixed acid medium, appropriate analysis conditions and analysis spectral lines are selected, an inductively coupled plasma atomic emission spectrometer is used for direct measurement, the mass concentration of an element to be measured is calculated according to a working curve method, and the measurement result is expressed by mass fraction. Analyzing an interference mechanism by observing the interference condition of the matrix on the emission intensity of the analysis element, thereby determining the matching condition of an internal standard element and the analysis element for correcting matrix interference: (1) establishing an analysis method for measuring the niobium element content of the aluminum-niobium alloy sample by using an inductively coupled plasma atomic emission spectrometry; (2) the method comprises the steps of dissolving an aluminum-niobium alloy sample, carrying out interference condition test on the measurement of niobium amount by aiming at different coexisting elements, optimizing the working state and working parameters of an instrument, determining the detection limit of the method, and investigating the precision of the method.
The same aluminum niobium alloy was subjected to measurement analysis in example 1, comparative example 1, and comparative example 2.
Example 1
In the embodiment, the method for measuring and analyzing the aluminum-niobium alloy by combining ICP-AES and a copper internal standard mainly comprises the following specific steps:
preparing a sample solution to be tested: weighing 0.10g (accurate to 0.0001g) of aluminum-niobium alloy sample, putting the aluminum-niobium alloy sample into a 150mL polyethylene beaker, adding 10mL deionized water and 20mL hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 1: 1: 1), and placing the aluminum-niobium alloy sample on a constant-temperature electric heating plate for constant-temperature heating; wherein the heating temperature is 70 ℃, after heating for 90 minutes, the aluminum-niobium alloy sample is completely dissolved, and then cooling is carried out, so as to obtain a sample solution.
Transferring the sample solution into a 250mL polyethylene volumetric flask, adding 30mL of copper internal standard solution (1000 mug/mL), adding water to constant volume, and shaking up to obtain a sample solution to be detected.
Preparing a working curve series solution: respectively taking 10mL, 15mL, 20mL, 25mL, 30mL and 35mL of 1000 mu g/mL Al standard solution, and sequentially adding the Al standard solution, the 15mL, the 25mL, the 30mL and the 35mL of 1000 mu g/mL Nb standard solution into a No. 1-6 250mL polyethylene volumetric flask; then, adding a copper internal standard solution (the volume of which is consistent with that of the copper internal standard solution added when the sample solution to be detected is prepared) and a hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (the volume of which is consistent with that of the mixed acid added when the sample solution to be detected is prepared) into No. 1-6 polyethylene volumetric flasks, diluting with water to constant volume scales, and uniformly mixing to obtain a working curve series solution. Wherein the mass concentrations (Al and Nb mass concentrations) of the elements to be detected in the working curve series solution are 0.04mg/mL, 0.06mg/mL, 0.08mg/mL, 0.10mg/mL, 0.12mg/mL and 0.14mg/mL in sequence.
Detection and analysis steps: sequentially placing the working curve series solution in a sample introduction system of an inductively coupled plasma spectrometer (Aglient 5800 (hydrofluoric acid resistant system)), measuring the intensity of the elements to be measured (aluminum and niobium elements) and the internal standard element, and drawing a working curve by taking the mass concentration of the mass elements to be measured as an abscissa and the intensity ratio of the elements to be measured and the internal standard element as an ordinate. And (3) measuring the strength ratio of the elements (aluminum and niobium elements) to be measured in the sample to be measured and the internal standard element in the sample in a sample introduction system of the inductively coupled plasma spectrometer, calculating the mass concentration of the elements to be measured in the sample solution to be measured through the working curve, and further calculating the mass fraction of the elements to be measured in the aluminum-niobium alloy sample.
In addition, in the detection and analysis step, Nb319.4nm is taken as a spectral line to be detected, and Cu327.3nm is taken as an internal standard spectral line; and (3) detecting Al394.4nm, Al396.1nm as spectral lines to be detected and Cu327.3nm as internal standard spectral lines (wherein, the analysis spectral line selection mainly selects spectral lines with small interference and high signal-to-back ratio, and selects spectral lines with good correlation with internal standard element spectral lines due to the addition of the internal standard).
The mass fraction of the elements to be detected in the aluminum-niobium alloy sample is calculated according to the following formula:
wherein rho is the mass concentration of an element to be detected in a sample solution to be detected, and the unit is mu g/mL;
v is the total volume of the sample solution to be detected, and the unit is mL;
m0the mass of the aluminum-niobium alloy sample is given in g.
Comparative example 1
Comparative example 1 measurement and analysis of aluminum-niobium alloy were performed directly by ICP-AES method (without internal standard), which mainly comprises the following steps:
preparing a sample solution to be tested: weighing 0.10g (accurate to 0.0001g) of aluminum-niobium alloy sample, putting the aluminum-niobium alloy sample into a 150mL polyethylene beaker, adding 10mL deionized water and 20mL hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 1: 1: 1), and placing the aluminum-niobium alloy sample on a constant-temperature electric heating plate for constant-temperature heating; wherein the heating temperature is 70 ℃, after heating for 90 minutes, the aluminum-niobium alloy sample is completely dissolved, and then cooling is carried out, so as to obtain a sample solution. And transferring the sample solution into a 250mL polyethylene volumetric flask, adding water to a constant volume, and shaking up to obtain a sample solution to be detected.
Preparing a working curve series solution: respectively taking 10mL, 15mL, 20mL, 25mL, 30mL and 35mL of 1000 mu g/mL Al standard solution, and sequentially adding the Al standard solution, the 15mL, the 25mL, the 30mL and the 35mL of 1000 mu g/mL Nb standard solution into a No. 1-6 250mL polyethylene volumetric flask; then, respectively adding hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (the volume of the mixed acid is consistent with that of the mixed acid added when the sample solution to be detected is prepared) into a No. 1-6 polyethylene volumetric flask, diluting with water to a constant volume scale, and uniformly mixing to obtain a working curve series solution. Wherein the mass concentrations (Al and Nb mass concentrations) of the elements to be detected in the working curve series solution are 0.04mg/mL, 0.06mg/mL, 0.08mg/mL, 0.10mg/mL, 0.12mg/mL and 0.14mg/mL in sequence.
Detection and analysis steps: sequentially putting the working curve series solution into a sample introduction system of an inductively coupled plasma spectrometer (Aglient 5800 type (hydrofluoric acid resistant system)), measuring the intensity of the elements to be measured (aluminum and niobium elements), and drawing a working curve by taking the mass concentration of the elements to be measured as an abscissa and the intensity of the elements to be measured as an ordinate. And (3) measuring the strength of elements (aluminum and niobium elements) to be measured in the sample in a sample introduction system of the inductively coupled plasma spectrometer, calculating the mass concentration of the elements to be measured in the sample solution to be measured through the working curve, and further calculating the mass fraction of the elements to be measured in the aluminum-niobium alloy sample.
Comparative example 2
Comparative example 2 measurement and analysis of the aluminum-niobium alloy by using the method of ICP-AES and the conventional internal standard mainly comprises the following steps:
preparing a sample solution to be tested: weighing 0.10g (accurate to 0.0001g) of aluminum-niobium alloy sample, putting the aluminum-niobium alloy sample into a 150mL polyethylene beaker, adding 10mL deionized water and 20mL hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (wherein the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is 1: 1: 1), and placing the aluminum-niobium alloy sample on a constant-temperature electric heating plate for constant-temperature heating; wherein the heating temperature is 70 ℃, after heating for 90 minutes, the aluminum-niobium alloy sample is completely dissolved, and then cooling is carried out, so as to obtain a sample solution.
Transferring the sample solution into a 250mL polyethylene volumetric flask, adding 30mL iron internal standard solution (1000 mug/mL), adding water to a constant volume, and shaking up to obtain a sample solution to be detected.
Preparing a working curve series solution: respectively taking 10mL, 15mL, 20mL, 25mL, 30mL and 35mL of 1000 mu g/mL Al standard solution, and sequentially adding the Al standard solution, the 15mL, the 25mL, the 30mL and the 35mL of 1000 mu g/mL Nb standard solution into a No. 1-6 250mL polyethylene volumetric flask; then, adding an iron internal standard solution (the volume of which is consistent with that of the iron internal standard solution added when the sample solution to be detected is prepared) and a hydrochloric acid-nitric acid-hydrofluoric acid mixed acid (the volume of which is consistent with that of the mixed acid added when the sample solution to be detected is prepared) into No. 1-6 polyethylene volumetric flasks, diluting with water to constant volume scales, and mixing uniformly to obtain a working curve series solution. Wherein the mass concentrations (Al and Nb mass concentrations) of the elements to be detected in the working curve series solution are 0.04mg/mL, 0.06mg/mL, 0.08mg/mL, 0.10mg/mL, 0.12mg/mL and 0.14mg/mL in sequence.
Detection and analysis steps: sequentially placing the working curve series solution in a sample introduction system of an inductively coupled plasma spectrometer (Aglient 5800 (hydrofluoric acid resistant system)), measuring the intensity of the elements to be measured (aluminum and niobium elements) and the internal standard element, and drawing a working curve by taking the mass concentration of the mass elements to be measured as an abscissa and the intensity ratio of the elements to be measured and the internal standard element as an ordinate. And (3) measuring the strength ratio of the elements (aluminum and niobium elements) to be measured in the sample to be measured and the internal standard element in the sample in a sample introduction system of the inductively coupled plasma spectrometer, calculating the mass concentration of the elements to be measured in the sample solution to be measured through the working curve, and further calculating the mass fraction of the elements to be measured in the aluminum-niobium alloy sample.
In addition, in the detection and analysis step, Nb319.4nm is taken as a spectral line to be detected, and Fe259.9nm is taken as an internal standard spectral line; and (3) Al394.4nm, Al396.1nm are spectral lines to be detected, Fe259.9nm is an internal standard spectral line, and detection is performed (here, the analysis spectral line selection mainly selects spectral lines with low interference and high signal-to-back ratio, and a spectral line with good correlation with an internal standard element spectral line is also selected due to the addition of the internal standard).
The results of the measurement and analysis of example 1, comparative example 1 and comparative example 2 are shown in table 1:
table 1 shows the effect of internal standard on data precision (n. 3)
The contents of aluminum and niobium in the aluminum-niobium alloy are high, and the greatest difficulty for ICP-AES detection is to detect elements with high contents, so that the problems of poor data stability and large deviation exist. Thus. In the embodiment 1 of the invention, an internal standard method is added to enable the element to be detected and the internal standard element to be in the same wave band spectral line, the detection and the exposure are carried out simultaneously, and the intensity value drift during the detection is calibrated by using the intensity ratio of the element to be detected and the internal standard element.
As can be seen from table 1: after the copper internal standard element is added, the stability of the test result is obviously superior to that of the test value of the comparative example 1 without the addition of the internal standard, and the precision of the data is improved. Referring to the data of comparative example 2, it can be seen that: and the stability of a test result is not obviously improved by selecting an iron internal standard element.
Therefore, the method provided by the embodiment of the invention can improve the accuracy and stability of the ICP-AES analysis on the aluminum-niobium alloy by selecting the copper internal standard element.
Example 2
This example mainly performs an interference experiment of the coexisting elements.
The aluminum-niobium alloy may contain the coexisting elements of iron, silicon, titanium, vanadium, molybdenum, and zirconium. If the interference line is overlapped with the analysis line, which causes data correction error, the data correction can be carried out by using an interference coefficient method. The interference factor is the ratio of the increase in the concentration of the analyte element caused by the interfering element to the concentration of the interfering element. The following experiments were performed: measuring the emission intensity In of 1mg/L pure aluminum and pure niobium standard solution and the interference intensity Im of 1000mg/mL interference elements In the pure aluminum, pure niobium and internal standard spectral line to be measured, calculating the interference coefficient formula (1), and correcting the formula (2). CT is the corrected real concentration, CS is the measured concentration when the element to be measured is interfered, and CD is the concentration of the interference element. The interference coefficient results are shown in table 2.
CT (CS-KCD) (2)
TABLE 2 interference coefficient determination test results
As can be seen from table 2: mo and Zr interfere with an Al396.1nm analysis spectral line, data needs to be calibrated, and other elements have no influence on the measurement results of the spectral line to be measured and the internal standard spectral line.
Example 3
The experiment was carried out according to the experimental method of example 1, and the linear regression equation obtained after the addition of the internal standard is shown in Table 3.
Table 3 shows the calibration curve
As can be seen from table 3: the quantitative analysis and determination method for the aluminum-niobium alloy provided by the embodiment of the invention has excellent stability and improves the correlation of a standard curve.
Example 4
This example mainly performs the precision, accuracy and recovery rate experiments. Specifically, an experimental sample was taken and measured according to the experimental method of example 1, and the results are shown in Table 4. The result shows that the RSD of the aluminum and the niobium is less than 0.10 after 10 times of measurement, and a better effect is achieved. A sample recovery rate test is carried out on the accuracy of the measured data, and the data recovery rate is stable between 98% and 102% as shown in Table 5, which shows that the method provided by the embodiment of the invention can be applied to the measurement of the aluminum-niobium intermediate alloy and has accurate results.
Table 4 precision test (n ═ 10)
TABLE 5 recovery test results
Example 5
In this example, the effect of the amount of mixed acid and the dissolution time of the aluminum niobium alloy sample on the test data is examined for the scheme of example 1:
(1) weighing a plurality of 30mg pure niobium substances in a plurality of beakers, respectively adding hydrofluoric acid into the beakers, wherein the dosage of the hydrofluoric acid is different, so as to carry out parallel comparison, and detecting the emission intensity of niobium in a dissolved aluminum-niobium alloy sample according to ICP-AES (inductively coupled plasma-atomic emission Spectrometry) to judge the dissolution degree of the sample; the results of the analysis are shown in FIG. 1.
As can be seen from fig. 1: after the dosage of the hydrofluoric acid reaches 4mL, the emission intensity of the niobium element does not change along with the increase of the dosage of the hydrofluoric acid, which shows that the niobium is completely dissolved and the solution is clear and not turbid after the dosage of the hydrofluoric acid reaches 4 mL.
(2) Weighing a plurality of 30mg pure Al substances in a plurality of beakers, respectively adding mixed acid of hydrochloric acid and nitric acid with the volume ratio of 1: 1 into the beakers, wherein the mixed acid is used in different amounts, so as to carry out parallel comparison, and detecting the emission intensity of Al in a dissolved aluminum-niobium alloy sample according to ICP-AES (inductively coupled plasma-atomic emission Spectrometry) to judge the dissolution degree of the sample; the results of the analysis are shown in FIG. 2.
As can be seen from fig. 2: when the mixed acid is added to reach 4mL, the emission intensity of the Al element is not changed, which shows that after the mixed acid is added to reach 4mL, the aluminum is completely dissolved, and the solution is clear and not turbid.
(3) Weighing a plurality of 30mg pure aluminum and niobium materials into a plurality of beakers (30 mg of aluminum and 30mg of niobium are put into each beaker), respectively adding 15mL of hydrofluoric acid-hydrochloric acid-nitric acid mixed acid into the beakers, placing the beakers on a constant-temperature electric hot plate (the heating temperature is 70 ℃), heating the beakers for different times, comparing parallel samples, and detecting the emission intensity of Al in the dissolved aluminum-niobium alloy sample according to ICP-AES (inductively coupled plasma-atomic emission Spectrometry) to judge the dissolution degree of the sample; the results of the analysis are shown in FIG. 3.
As can be seen from fig. 3: when the emission intensity of the Al element and the niobium element is constant after the sample dissolving time (heating time) is more than 90 minutes, the following results are obtained: after a consistent amount (15mL) of mixed acid of hydrofluoric acid, hydrochloric acid and nitric acid is added, the mixture is placed on a constant-temperature electric heating plate, and after the mixture is heated at 70 ℃ for 90 minutes, a sample is completely dissolved, insoluble substances and turbidity do not exist, and the mixture is diluted to a 250mL polyethylene volumetric flask, so that the chemical property is stable and no precipitation exists.
In conclusion, the ICP-AES method is applied to sample analysis of the aluminum-niobium alloy, the copper internal standard element is selected, and the accurate determination of the high-content niobium and aluminum elements has extremely important influence on improving the product quality and promoting the development of aluminum alloy materials in China. Meanwhile, the method solves the problem of the method deficiency of the ICP-AES method for simultaneously analyzing the niobium and aluminum elements in the aluminum intermediate alloy, improves the inadaptable current situation in the technical aspect of GB/T20975 and 2008 'chemical analysis method for aluminum and aluminum alloy', and meets the requirements of production enterprises and downstream customers on accurate detection of large-batch aluminum-niobium alloys.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. The quantitative analysis and determination method of the aluminum-niobium alloy is characterized by comprising the following steps of:
preparing a sample solution to be tested: preparing an aluminum-niobium alloy sample into a sample solution to be detected; wherein the to-be-detected sample solution also contains a copper internal standard element;
preparing a working curve series solution: preparing a working curve series solution with gradient concentration of the element to be detected; the element to be detected is one or two of aluminum element and niobium element; wherein the working curve series solution also contains a copper internal standard element;
detection and analysis steps: and measuring and analyzing the working curve series solution and the sample solution to be measured by using an inductively coupled plasma spectrometer, and calculating the content of the element to be measured in the aluminum-niobium alloy sample.
2. The method for quantitative analysis and determination of an aluminum-niobium alloy according to claim 1, wherein the step of preparing a sample solution to be tested comprises:
mixing an aluminum-niobium alloy sample, water and mixed acid, and heating at a set temperature to completely dissolve the aluminum-niobium alloy sample to obtain a sample solution;
adding a copper internal standard solution into the sample solution, and fixing the volume to a set volume to obtain a sample solution to be measured; preferably, after the copper internal standard solution is added into the sample solution, water is added into the sample solution to be constant to a set volume.
3. The method for the quantitative analysis and determination of an aluminum-niobium alloy according to claim 2,
in the sample solution: the mass of the aluminum-niobium alloy sample is 0.10 +/-0.0001 g, and the volume of the water is 5-20 mL; the volume of the mixed acid is more than or equal to 15mL, preferably less than or equal to 25 mL;
preferably, the water is deionized water;
preferably, the mixed acid is mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid; further preferably, in the mixed acid: the volume ratio of the hydrochloric acid to the nitric acid to the hydrofluoric acid is (0.5-1.5) to (0.5-1.5), preferably 1: 1;
preferably, the set temperature is 60-80 ℃ and the heating time is 90 minutes or more.
4. The method for quantitative analysis and determination of aluminum-niobium alloy according to claim 3, wherein if the inductively coupled plasma emission spectrometer is an Aglient5800 type inductively coupled plasma emission spectrometer, the amount of the standard solution with copper internal standard is such that the content of the copper internal standard element in the sample solution to be determined is 30mg ± 0.1 mg.
5. The method for the quantitative analysis and determination of an aluminum-niobium alloy according to any one of claims 1 to 4, wherein in the step of preparing the working curve series solution:
the working curve series solution comprises a plurality of working curve solutions, and the concentration of the element to be detected in the working curve solutions is sequentially increased; wherein the concentration of each element to be detected in the solution of the first working curve is 0.03-0.05mg/mL, preferably 0.04 mg/mL; preferably, the difference value of each element to be detected concentration of the solution of the latter working curve and the solution of the former working curve is 0.015-0.025mg/mL, and preferably 0.02 mg/mL;
preferably, the series of working curve solutions comprises 6 working curve solutions.
6. The method for quantitative analysis and determination of an aluminum-niobium alloy according to claim 5, wherein the mass of the copper internal standard element in each of the working curve solutions is the same as the mass of the copper internal standard element in the sample solution to be tested.
7. The method for quantitative analysis and determination of aluminum-niobium alloy according to claim 5, wherein each of the working curve solutions is prepared from a standard solution of an element to be measured, a standard solution of a copper internal standard, a mixed acid and water;
the volume of the working curve solution is consistent with that of the sample solution to be detected;
the volume of the mixed acid in the working curve solution is the same as that of the mixed acid in the sample solution to be detected;
the volume of the copper internal standard solution in the working curve solution is the same as that of the copper internal standard solution in the sample solution to be detected;
the standard solution of the element to be detected comprises one or two of an aluminum standard solution and a niobium standard solution;
preferably, the preparation steps of each working curve solution are as follows: and mixing the element standard solution to be measured, the copper internal standard solution and the mixed acid, and then adding water into the mixture to fix the volume to a set volume.
8. The method for the quantitative analysis and determination of an aluminum-niobium alloy according to any one of claims 1 to 7, wherein in the detecting and analyzing step:
detecting the working curve series solution by using an inductively coupled plasma spectrometer, measuring the intensity of the element to be measured and the copper internal standard element, and drawing a working curve by using the mass concentration of the element to be measured as a horizontal coordinate and the intensity ratio of the element to be measured and the internal standard element as a vertical coordinate;
and detecting the sample solution to be detected by adopting an inductively coupled plasma spectrometer, determining the strength ratio of the element to be detected and the internal standard element in the aluminum-niobium alloy sample, calculating the mass concentration of the element to be detected in the sample solution to be detected through the working curve, and further calculating the mass fraction of the element to be detected in the aluminum-niobium alloy sample.
9. The method for quantitative analysis and determination of an aluminum-niobium alloy according to claim 8, wherein the mass fraction of the element to be measured in the aluminum-niobium alloy sample is calculated according to the following formula:
wherein rho is the mass concentration of an element to be detected in a sample solution to be detected, and the unit is mu g/mL;
v is the total volume of the sample solution to be detected, and the unit is mL;
m0the mass of the aluminum-niobium alloy sample is given in g.
10. The method for quantitative analysis and determination of an aluminum-niobium alloy according to claim 8, wherein in the detecting and analyzing step:
if the element to be detected is niobium, taking Nb319.4nm as a spectral line to be detected and Cu327.3nm as an internal standard spectral line;
and if the element to be detected is aluminum, taking Al394.4nm, Al396.1nm as a spectral line to be detected and Cu327.3nm as an internal standard spectral line.
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