CN114354298A - Method for determining ruthenium content in zirconium alloy - Google Patents
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Abstract
The invention discloses a method for measuring ruthenium content in zirconium alloy, which comprises the following steps: carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a liquid to be detected; adding an acidic reagent into a plurality of parts of high-purity zirconium to carry out chemical reaction to obtain a plurality of parts of matrix solution; adding ruthenium standard solutions with different concentrations into a plurality of parts of the matrix solution respectively to obtain a calibration solution; establishing a calibration curve of the characteristic spectrum intensity and the concentration of the ruthenium element in the calibration solution; and measuring the characteristic spectrum intensity of the ruthenium element in the liquid to be detected, and obtaining the concentration of the ruthenium element in the liquid to be detected based on the calibration curve. The invention provides a method for measuring the content of ruthenium in zirconium alloy, which improves the measurement of the content of the element in the zirconium alloy at present, overcomes the matrix effect and ensures that the measurement precision of the content of the ruthenium in the zirconium alloy meets the requirement of zirconium alloy detection in industry.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for determining ruthenium content in zirconium alloy.
Background
Because of its excellent corrosion resistance and good mechanical and heat transfer properties, zirconium alloy is widely used in petrochemical industry, such as pressure vessels, heat exchangers, pipelines, tanks, shafts, mixers and other mechanical equipment, valves, pumps, sprayers, trays, demisters, tower liners, and the like.
At present, the domestic zirconium alloy chemical analysis method GB/T13747 and the publicly reported chemical analysis methods have no determination method of ruthenium element in zirconium alloy, and the main technical difficulties are as follows:
(1) zirconium alloy is usually dissolved by using acid liquor so as to measure the elements in the zirconium alloy, however, the chemical property of ruthenium element is very stable, when the temperature reaches 100 ℃, ruthenium still has resistance to common acids including aqua regia and resistance to hydrofluoric acid and phosphoric acid, and the conventional dissolving means cannot completely dissolve zirconium alloy samples containing ruthenium, so that the content of ruthenium element in the zirconium alloy is difficult to effectively measure.
(2) At present, most trace elements in zirconium alloy mostly adopt inductively coupled plasma emission spectrometry, and because zirconium is a spectrum enrichment element, the detection of the element is greatly influenced by the matrix effect, so that the accuracy and precision of the measurement result are not good.
Disclosure of Invention
The embodiment of the invention aims to provide a method for measuring the ruthenium content in a zirconium alloy, so that the detection of elements in the zirconium alloy is more comprehensive, the method ensures the accuracy of the measurement of the ruthenium content in the zirconium alloy, and the detection accuracy can meet the requirement of the zirconium alloy detection in the industry.
In order to solve the above technical problem, an embodiment of the present invention provides a method for determining a ruthenium content in a zirconium alloy, including: carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a liquid to be detected; adding an acidic reagent into a plurality of parts of high-purity zirconium to carry out chemical reaction to obtain a plurality of parts of matrix solution; adding ruthenium standard solutions with different concentrations into a plurality of parts of matrix solutions respectively to obtain calibration solutions; establishing a calibration curve of the characteristic spectrum intensity and the concentration of the ruthenium element in the calibration solution; and measuring the characteristic spectrum intensity of the ruthenium element in the liquid to be detected, and obtaining the concentration of the ruthenium element in the liquid to be detected based on the calibration curve.
Further, before the sample to be detected and the acidic reagent are subjected to a chemical reaction to obtain a solution to be detected, the method further comprises the following steps: and (3) pretreating a sample to be detected, wherein the pretreatment comprises machining, surface pickling, soaking and drying.
Further, the acidic reagent comprises water and hydrofluoric acid-nitric acid composite acid liquid; the volume ratio of the water to the hydrofluoric acid-nitric acid composite acid liquid is 1:1-1: 1.5.
Further, the ratio of the volume of the acidic reagent to the mass of the sample to be detected is: 8:1-24:1 (mL/g); the mass of the sample to be detected is the same as that of each high-purity zirconium.
Further, the hydrofluoric acid-nitric acid composite acid liquid contains 12-16% of hydrofluoric acid and 5-9% of nitric acid by mass.
Further, the method for obtaining the liquid to be detected by carrying out chemical reaction on the sample to be detected and the acidic reagent comprises the following steps: carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a solid-liquid mixture; and (4) digesting the solid-liquid mixture by using a microwave digestion instrument to obtain a liquid to be detected.
Further, the working parameters of the microwave digestion instrument are as follows: the temperature is 120-180 ℃, the pressure is 30-60 bar, and the time is 1-2 h.
Further, measuring the characteristic spectrum intensity of the ruthenium element in the liquid to be detected and the calibration solution by adopting an inductively coupled plasma emission spectrometer; the wavelength of the spectral line of the inductively coupled plasma emission spectrometer is 240.272 nm.
Further, the operating parameters of the inductively coupled plasma emission spectrometer are as follows: the radio frequency power is 1300W-1400W, the cooling air flow is 10L/min-12L/min, the auxiliary air flow is 0.6L/min-1L/min, the atomization air flow is 0.6L/min-0.9L/min, and the pump speed of the peristaltic pump is 20 rpm-40 rpm.
Further, the linear correlation coefficient of the characteristic spectral intensity of the ruthenium element in the calibration curve with the concentration is equal to or greater than 0.998.
The technical scheme of the embodiment of the invention has the following beneficial technical effects:
the method overcomes the matrix effect in the detection process of the zirconium alloy element and ensures the accuracy of the determination of the ruthenium element in the zirconium alloy.
Drawings
Fig. 1 is a calibration graph of characteristic spectrum intensity and concentration of ruthenium element in a calibration solution according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In an alternative embodiment, the step of the method of determining ruthenium content in a zirconium alloy comprises:
(1) preparing a liquid to be detected: and adding an acidic reagent into the sample to be detected to obtain a liquid to be detected, wherein the sample to be detected is zirconium alloy, and the acidic reagent is hydrofluoric acid-nitric acid composite acid liquid.
(2) Preparation of calibration solutions: respectively adding an acidic reagent into a plurality of parts of high-purity zirconium to obtain a plurality of parts of matrix solutions; and adding ruthenium standard solutions with different concentrations into the multiple parts of matrix solutions respectively to obtain multiple parts of calibration solutions with different ruthenium contents.
(3) Establishing a calibration curve of the characteristic spectrum intensity and the concentration of the ruthenium element: and measuring the characteristic spectrum intensity of the ruthenium element in a plurality of calibration solutions with different ruthenium contents by using an inductively coupled plasma emission spectrometer, and inputting the respective characteristic spectrum intensity values in the plurality of calibration solutions and ruthenium concentration values corresponding to the characteristic spectrum intensity values by using a computer to obtain a calibration curve of the characteristic spectrum intensity and the concentration of the ruthenium element.
(4) Calculating the content of the ruthenium element in the liquid to be detected: and measuring the characteristic spectrum intensity of the ruthenium element in the liquid to be detected by adopting an inductively coupled plasma emission spectrometer, inputting the intensity value into a computer, and calculating a concentration value corresponding to the intensity value by the computer based on a calibration curve so as to obtain the concentration of the ruthenium element in the liquid to be detected.
Optionally, the sample to be tested and the acid reagent are subjected to chemical reaction under the conditions of high temperature and high pressure, so that the sample to be tested is completely dissolved.
In another optional embodiment, when the reaction between the sample to be detected and the acidic reagent is observed to be nearly stopped by naked eyes, the microwave digestion instrument is adopted for digestion, so that the sample to be detected is completely dissolved.
In some embodiments, the pre-treating the sample to be tested comprises: roughly processing a sample to be detected by a lathe, and shearing by using a wire cutter to obtain a blocky sample to be detected; and (3) pickling the massive sample to be detected with hydrofluoric acid-nitric acid pickling solution to remove surface oxide skin, soaking with an organic reagent, and drying for later use.
Wherein, the hydrofluoric acid-nitric acid pickling solution for pickling contains 2-7% of hydrofluoric acid by mass and 20-50% of nitric acid by mass.
In a specific embodiment, the solution to be detected, the matrix solution and the calibration solution are obtained by using purified water to perform constant volume and shaking up.
In some embodiments, the ruthenium standard solution is 0mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 5mg/L, 10mg/L, respectively.
Example one
The method for determining the ruthenium content in the zirconium alloy comprises the following steps:
firstly, roughly processing zirconium alloy by a lathe, shearing by using a wire cutter to obtain a blocky sample to be detected, pickling the blocky sample to be detected by using hydrofluoric acid-nitric acid pickling solution to remove oxide skin, soaking the sample in an organic reagent, and drying for later use;
wherein, the mass percentage of hydrofluoric acid in the pickling solution is 3%, and the mass percentage of nitric acid is 40%.
Weighing a sample with the mass of 1g, accurately measuring the sample to 0.0010g, placing the sample in a polytetrafluoroethylene digestion tank special for microwave digestion, adding water and hydrofluoric acid-nitric acid composite acid liquid with the volume of 10mL into a beaker, placing the digestion tank in a microwave digestion instrument for high-temperature high-pressure dissolution when the reaction is nearly stopped, cooling, and then, adding pure water to a constant volume of 100mL and shaking up to obtain a liquid to be detected;
wherein, the microwave digestion instrument has the following setting parameters: the temperature is 130 ℃, the pressure is 30bar, and the time is 2 h; the hydrofluoric acid-nitric acid composite acid liquid contains 14% by mass of hydrofluoric acid and 6% by mass of nitric acid.
And step three, respectively placing 6 parts of high-purity zirconium with the mass of 1g in 6 hydrofluoric acid-resistant beakers, adding 10mL of water and hydrofluoric acid-nitric acid composite acid liquor for dissolving to obtain 6 parts of matrix solution, then taking 6 volumetric flasks, respectively transferring each part of matrix solution and ruthenium standard solution with known measurement into 6 volumetric flasks, respectively metering to 100mL by using pure water, shaking uniformly to obtain calibration solutions with different concentrations, wherein the concentrations of the ruthenium standard solution are respectively 0mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 5mg/L and 10 mg/L.
Step four, measuring the characteristic spectral intensity of the ruthenium element in the calibration solution with different concentrations in the step three one by one at 240.272nm by adopting an inductively coupled plasma emission spectrometer, establishing a calibration curve of the spectral intensity and the ruthenium concentration, and knowing from figure 1 that the linear correlation coefficient of the calibration curve is more than or equal to 0.998;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1350W, the cooling air flow is 10min, the auxiliary air flow is 0.7L/min, the atomization air flow is 0.6L/min, and the pump speed of the peristaltic pump is 20 rpm.
Step five, measuring the characteristic spectrum intensity of the liquid to be detected in the step two at 240.272nm by using an inductively coupled plasma emission spectrometer, then calculating the concentration of the liquid to be detected according to the calibration curve of the intensity and the concentration established in the step four, and finally calculating the mass content of ruthenium element in the zirconium alloy;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1350W, the cooling air flow is 10min, the auxiliary air flow is 0.7L/min, the atomization air flow is 0.6L/min, and the pump speed of the peristaltic pump is 20 rpm.
In this example, the content of ruthenium in the solution to be detected was determined according to the calibration curve, three experiments were performed in parallel, and the average value was calculated as the determination result, as shown in Table 1
Table 1 example 1 measurement results
Example two
The method for determining the ruthenium content in the zirconium alloy comprises the following steps:
firstly, roughly processing zirconium alloy by a lathe, shearing by using a wire cutter to obtain a blocky sample to be detected, pickling the sample to be detected by using hydrofluoric acid-nitric acid pickling solution to remove oxide skin, soaking the sample by using an organic reagent, and drying the sample for later use;
wherein, the mass percentage of hydrofluoric acid in the pickling solution is 5 percent, and the mass percentage of nitric acid is 30 percent;
weighing a sample with the mass of 0.5g, accurately weighing the sample to 0.0010g, adding 5mL of water and hydrofluoric acid-nitric acid composite acid solution into a beaker in a polytetrafluoroethylene digestion tank special for microwave digestion, placing the digestion tank in a microwave digestion instrument for high-temperature high-pressure dissolution when the reaction is nearly stopped, cooling, and uniformly shaking to obtain a solution to be detected, wherein the volume of the solution is 50 mL;
wherein, the microwave digestion instrument has the following setting parameters: the temperature is 150 ℃, the pressure is 50bar, and the time is 1.5 h; the mass percentage of the hydrofluoric acid in the hydrofluoric acid-nitric acid composite acid liquid is 15%, and the mass percentage of the nitric acid is 7%.
And step three, respectively placing 6 parts of high-purity zirconium with the mass of 0.5g in 6 hydrofluoric acid-resistant beakers, adding 5mL of water and hydrofluoric acid-nitric acid composite acid liquor for dissolving to obtain 6 parts of matrix solution, then taking 6 volumetric flasks, respectively transferring each part of matrix solution and the measured ruthenium standard solution into the 6 volumetric flasks, respectively metering to 50mL by using pure water, shaking uniformly to obtain ruthenium calibration solutions with different concentrations, wherein the concentrations of the ruthenium standard solutions are respectively 0mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 5mg/L and 10 mg/L.
Step four, measuring the characteristic spectral intensity of ruthenium in the calibration solution with different concentrations in step three one by one at 240.272nm by adopting an inductively coupled plasma emission spectrometer, establishing a calibration curve of the spectral intensity and the ruthenium concentration, and knowing from figure 1 that the linear correlation coefficient of the calibration curve is more than or equal to 0.998;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1400W, the cooling air flow is 11min, the auxiliary air flow is 0.8L/min, the atomization air flow is 0.8L/min, and the pump speed of the peristaltic pump is 30 rpm.
Step five, measuring the characteristic spectrum intensity of the liquid to be detected in the step two at 240.272nm by using an inductively coupled plasma emission spectrometer, then calculating the concentration of the liquid to be detected according to the calibration curve of the intensity and the concentration established in the step four, and finally calculating the mass content of ruthenium element in the zirconium alloy;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1400W, the cooling air flow is 11min, the auxiliary air flow is 0.8L/min, the atomization air flow is 0.8L/min, and the pump speed of the peristaltic pump is 30 rpm.
In this example, the content of ruthenium in the solution to be detected was determined according to the calibration curve, three experiments were performed in parallel, and the average value was calculated as the determination result, as shown in Table 2
Table 2 example 2 measurement results
EXAMPLE III
The method for determining the ruthenium content in the zirconium alloy comprises the following steps:
firstly, roughly processing zirconium alloy by a lathe, shearing by using a wire cutter to obtain a blocky sample to be detected, pickling the sample to be detected by using hydrofluoric acid-nitric acid pickling solution to remove oxide skin, soaking the sample by using an organic reagent, and drying the sample for later use;
wherein the acid washing solution contains 6 mass percent of hydrofluoric acid and 45 mass percent of nitric acid.
Weighing a sample with the mass of 1g, accurately measuring the sample to 0.0020g, placing the sample in a polytetrafluoroethylene digestion tank special for microwave digestion, adding water and hydrofluoric acid-nitric acid composite acid liquid with the volume of 10mL into a beaker, placing the digestion tank in a microwave digestion instrument for high-temperature high-pressure dissolution when the reaction is nearly stopped, cooling, and then, fixing the volume to 100mL by using pure water and shaking up to obtain a liquid to be detected;
wherein, the microwave digestion instrument has the following setting parameters: the temperature is 160 ℃, the pressure is 55bar, and the time is 1 h; the hydrofluoric acid-nitric acid composite acid liquid contains 16% by mass of hydrofluoric acid and 8% by mass of nitric acid.
And step three, respectively placing 6 parts of high-purity zirconium with the mass of 1g in 6 hydrofluoric acid-resistant beakers, adding 10mL of water and hydrofluoric acid-nitric acid composite acid liquor for dissolving to obtain 6 parts of matrix solution, then taking 6 volumetric flasks, respectively transferring each part of matrix solution and the measured ruthenium standard solution into the 6 volumetric flasks, respectively metering the volume to 100mL by using pure water, shaking up to obtain calibration solutions with different concentrations, wherein the concentrations of the ruthenium standard solutions are respectively 0mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 5mg/L and 10 mg/L.
Step four, measuring the characteristic spectral intensity of the ruthenium element in the calibration solution with different concentrations in the step three one by one at 240.272nm by adopting an inductively coupled plasma emission spectrometer, establishing a calibration curve of the spectral intensity and the ruthenium concentration, and knowing from figure 1 that the linear correlation coefficient of the calibration curve is more than or equal to 0.998;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1350W, the cooling air flow is 12min, the auxiliary air flow is 0.9L/min, the atomization air flow is 0.8L/min, and the pump speed of the peristaltic pump is 40 rpm.
Step five, measuring the characteristic spectrum intensity of the liquid to be detected in the step two at 240.272nm by using an inductively coupled plasma emission spectrometer, then calculating the concentration of the liquid to be detected according to the calibration curve of the intensity and the concentration established in the step four, and finally calculating the mass content of ruthenium element in the zirconium alloy;
the inductively coupled plasma emission spectrometer has the following working parameters: the radio frequency power is 1350W, the cooling air flow is 12min, the auxiliary air flow is 0.9L/min, the atomization air flow is 0.8L/min, and the pump speed of the peristaltic pump is 40 rpm.
In this example, the content of ruthenium in the solution to be detected was determined according to the calibration curve, three experiments were performed in parallel, and the average value was calculated as the determination result, as shown in Table 3
Table 3 example 3 measurement results
The invention adopts a standard recovery rate test to verify the accuracy of the method. Sample solutions were prepared according to steps one through two, and standard solutions of different concentrations were added, with the results of recovery on addition of standard being shown in table 4.
TABLE 4 results of recovery with addition of standard
As is clear from Table 4, the recovery rate was from 95% to 105, which indicates that the accuracy of the present invention is high and the measurement result is accurate.
The invention adopts independent determination of 3 days samples, independent determination 7 times per day, and calculation of relative standard deviation to verify the precision of the method. Sample solutions were prepared according to steps one through two, and the results of the measurements are shown in Table 5.
TABLE 5 stability results
As can be seen from Table 5, the relative standard deviation is less than or equal to 10%, thus demonstrating that the method for determining the ruthenium content in the zirconium alloy provided by the invention has good precision and stable measurement result.
The embodiment of the invention aims to protect a method for measuring the content of ruthenium in zirconium alloy, which has the following effects:
1. the invention adopts a microwave digestion method, and solves the problem that the sample cannot be dissolved completely in a common dissolving mode.
2. The method adopts the high-purity zirconium bottom as the matrix of the calibration solution, effectively reduces the interference of matrix effect on the element measurement, and improves the accuracy of the ruthenium element content measurement.
3. The invention establishes a method for measuring the ruthenium content in the zirconium alloy, fills the blank of the prior art, and meets the detection standard of the industrial zirconium alloy.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (10)
1. A method of determining ruthenium content in a zirconium alloy, the method comprising:
carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a liquid to be detected;
adding the acidic reagent into a plurality of parts of high-purity zirconium to carry out chemical reaction to obtain a plurality of parts of matrix solution;
adding ruthenium standard solutions with different concentrations into a plurality of parts of the matrix solution respectively to obtain a calibration solution;
establishing a calibration curve of the characteristic spectrum intensity and the concentration of the ruthenium element in the calibration solution;
and measuring the characteristic spectrum intensity of the ruthenium element in the liquid to be detected, and obtaining the concentration of the ruthenium element in the liquid to be detected based on the calibration curve.
2. The method of claim 1,
before the chemical reaction is carried out between the sample to be detected and the acidic reagent to obtain the liquid to be detected, the method further comprises the following steps: and pretreating the sample to be detected, wherein the pretreatment comprises machining, surface pickling, soaking and drying.
3. The method of claim 1,
the acidic reagent comprises water and hydrofluoric acid-nitric acid composite acid liquid;
the volume ratio of the water to the hydrofluoric acid-nitric acid composite acid liquid is 1:1-1: 1.5.
4. The method of claim 1,
the ratio of the volume of the acidic reagent to the mass of the sample to be detected is 8:1-24:1 (mL/g);
the mass of the sample to be detected is the same as that of each part of high-purity zirconium.
5. The method of claim 3,
the hydrofluoric acid-nitric acid composite acid liquid contains 12-16% of hydrofluoric acid and 5-9% of nitric acid by mass percent.
6. The method of claim 1,
the method for carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a liquid to be detected comprises the following steps:
carrying out chemical reaction on a sample to be detected and an acidic reagent to obtain a solid-liquid mixture;
and (4) digesting the solid-liquid mixture by using a microwave digestion instrument to obtain a liquid to be detected.
7. The method according to claim 6, wherein the operating parameters of the microwave digestion instrument are: the temperature is 120-180 ℃, the pressure is 30-60 bar, and the time is 1-2 h.
8. The method of claim 1,
measuring the characteristic spectral intensity of the ruthenium element in the liquid to be detected and the calibration solution by using an inductively coupled plasma emission spectrometer;
the wavelength of a spectral line of the inductively coupled plasma emission spectrometer is 240.272 nm.
9. The method of claim 8,
the working parameters of the inductively coupled plasma emission spectrometer are as follows: the radio frequency power is 1300W-1400W, the cooling air flow is 10L/min-12L/min, the auxiliary air flow is 0.6L/min-1L/min, the atomization air flow is 0.6L/min-0.9L/min, and the pump speed of the peristaltic pump is 20 rpm-40 rpm.
10. The method of claim 1,
the linear correlation coefficient of the characteristic spectrum intensity and the concentration of the ruthenium element in the calibration curve is more than or equal to 0.998.
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