CN114252432A - Method for measuring gallium content in antibacterial stainless steel - Google Patents
Method for measuring gallium content in antibacterial stainless steel Download PDFInfo
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Abstract
The invention belongs to the technical field of alloy macroelement analysis, and particularly provides a method for determining gallium content in antibacterial stainless steel, so as to fill the blank of the existing method for detecting gallium content in antibacterial stainless steel. The method is characterized in that aqua regia is used for dissolving gallium-containing antibacterial stainless steel, iron matrix interference is eliminated through a matrix matching method, matrix blank is used as a standard working curve blank for eliminating iron spectral line interference, and an analysis detection method for measuring gallium content in the stainless steel through inductively coupled plasma atomic emission spectrometry is established. The method is simple and convenient to operate, the precision of the test result is good, the accuracy is high, and the detection requirement of gallium in the novel antibacterial stainless steel can be met.
Description
Technical Field
The invention belongs to the technical field of alloy macroelement analysis, and particularly provides a method for determining gallium content in antibacterial stainless steel.
Background
The antibacterial stainless steel is prepared by adding a certain amount of antibacterial metal elements into common stainless steel, and uniformly distributing the elements in the material through a special heat treatment processing technology, so that the antibacterial stainless steel has an antibacterial function. The gallium-containing antibacterial stainless steel is characterized in that 0.2-3.0 wt% of metal gallium with the function of inhibiting bacterial reproduction is added on the basis of the traditional copper-containing antibacterial stainless steel, so that the metal gallium and copper are synergistically acted to jointly resist bacteria, and the antibacterial performance of the material is improved. The content of the gallium element has a remarkable influence on the antibacterial performance of the stainless steel, so that the content needs to be accurately measured.
At present, no detection method for the constant gallium in the stainless steel is reported. Methods for measuring the gallium content in other materials include rhodamine B colorimetry, EDTA complex titration, atomic absorption, inductively coupled plasma mass spectrometry, inductively coupled plasma atomic emission spectrometry and the like. The colorimetric method and the spectrophotometry have the disadvantages of complicated operation steps, long analysis period and difficulty in meeting the requirement of rapid detection; the atomic absorption method and the inductively coupled plasma mass spectrometry are mainly used for detecting trace elements and are not suitable for constant analysis. The inductively coupled plasma atomic emission spectrometry has the advantages of high analysis speed, high accuracy, wide dynamic linear range, capability of simultaneously measuring multiple elements and the like, and is widely used for analyzing and detecting the macroelements. The existing report of measuring the constant gallium in the copper indium gallium selenide target material and the zinc oxide powder by the inductively coupled plasma atomic emission spectrometry is available, but the components of the materials are greatly different from stainless steel, the sample dissolving method and the interference condition of the spectral line are possibly different, and the existing method cannot be carried out. At present, an analysis method for measuring the gallium content in the antibacterial stainless steel is still blank.
Disclosure of Invention
The invention aims to provide a method for measuring gallium content in antibacterial stainless steel, which adopts inductively coupled plasma atomic emission spectrometry capable of accurately and quickly measuring the gallium content in the antibacterial stainless steel so as to fill up the technical blank of analyzing and detecting the gallium content in the stainless steel, wherein the measurement range is as follows: 0.10 wt% -5.00 wt%.
The technical scheme of the invention is as follows:
a method for measuring the content of gallium in antibacterial stainless steel comprises the following steps:
(1) measuring on an inductively coupled plasma atomic emission spectrometer in an axial direction under the selected working parameters of the instrument and the wavelength of a gallium analysis line;
(2) reagent
(2.1) a gallium single element standard solution with the concentration of 1000 mug/mL;
(2.2) iron single element standard solution with concentration of 10 mg/mL: is prepared by dissolving metal iron with the purity not less than 99.99 wt% by hydrochloric acid and nitric acid;
(2.3) hydrochloric acid, [ rho ] 1.19g/mL, CMOS grade;
(2.4) nitric acid, [ rho ] 1.42g/mL, CMOS grade;
(2.5) the test water is secondary water, and the conductivity at 25 ℃ is less than or equal to 0.10 mS/m;
(3) selection of analytical lines
Selecting a gallium element spectral line of 417.206 nm;
(4) correction of disturbances in analysis lines
Eliminating interference of an iron matrix by a matrix matching method, and deducting interference of a ferrographic line by taking a matrix blank as a standard working curve blank;
(5) measurement of
(5.1) preparation of test solution
Weighing 0.1000g of a sample to be detected in a 50mL beaker, adding 1mL of nitric acid and 3mL of hydrochloric acid, heating at the low temperature of 60 ℃ until the nitric acid and the hydrochloric acid are completely dissolved, taking down and cooling to the room temperature, transferring the solution to a 100mL volumetric flask, diluting the solution to a scale with water, and uniformly mixing the solution to be detected;
(5.2) preparation of Standard working Curve solution
Firstly, respectively transferring 7mL of the iron single element standard solution obtained in the step (2.2) into 5 100mL volumetric flasks, and respectively adding 1mL of nitric acid and 3mL of hydrochloric acid into each volumetric flask; then, adding gallium single element standard solutions with different amounts into the volumetric flasks respectively, diluting the solutions to a scale with water, and uniformly mixing the solutions; the percentage contents of gallium in the series of standard working curve solutions, which is equivalent to 0.1000g of a sample, are respectively as follows: 0 (matrix blank), 0.1 wt%, 0.5 wt%, 1 wt%, 5 wt%;
(5.3) measurement
Under the selected working condition of the instrument and the wavelength of the gallium analysis line, sequentially measuring the spectral intensity of gallium in the standard working curve solution in the step (5.2) according to the sequence of the concentration from low to high, repeating each solution for 2 times, and calculating the average value of the solution; and (3) drawing a standard working curve of the gallium and calculating a correlation coefficient of the standard working curve by taking the average value of the spectral intensity minus the average value of the spectral intensity of the blank solution of the substrate as a vertical coordinate and the percentage content of the gallium as a horizontal coordinate, wherein the correlation coefficient is not less than 0.999.
After the step (5.3), when the linearity of the working curve meets the requirement, measuring the gallium element in the test solution in the step (5.1), repeating the measurement for 2 times, and calculating the average value; and subtracting the average value of the spectrum intensity of the matrix blank solution from the average value of the spectrum intensity of the sample to obtain the net spectrum intensity, and checking the percentage content of gallium in the sample from the standard working curve.
In the method for measuring the gallium content in the antibacterial stainless steel, in the step (1), the optimized working parameters of the inductively coupled plasma atomic emission spectrometer are as follows: the power of the high-frequency generator is 1.2 kW; the plasma gas flow is 16 mL/min; the flow rate of the atomized gas is 1.0 mL/min; the auxiliary gas flow is 0.2 mL/min; the lifting amount of the solution is 1.5 mL/min; the integration time is 2-5 s; the observation direction is axial; the height of observation was 11 mm.
The invention has the advantages and beneficial effects that:
1. the invention establishes a detection method for measuring the gallium content in the antibacterial stainless steel by using an inductively coupled plasma atomic emission spectrometry, and fills the blank of the existing detection method for the gallium content in the antibacterial stainless steel;
2. the invention eliminates the interference of the iron matrix by a matrix matching method, and the blank of the matrix is used as the blank of the standard working curve to deduct the interference of the iron spectrum line, thereby improving the accuracy and precision of measurement;
3. the method has the advantages of simple operation, high sensitivity, good reproducibility, high precision, good accuracy and wide linear range, and does not influence the determination of other elements.
Drawings
FIG. 1 is a standard operating curve for gallium plotted in example 1. In the figure, the abscissa ωGaRepresents the gallium content (%) in mass% and the ordinate Intensity represents the relative Intensity (cps).
Detailed Description
The present invention will be described in further detail below with reference to examples.
Example 1
In this embodiment, the method for determining the content of gallium in 304 antimicrobial stainless steel is as follows:
(1) the measurement is carried out on an inductively coupled plasma atomic emission spectrometer (Optima7300DV, Perkin Elemer company in USA), and the optimized working conditions of the instrument are as follows: the power of the high-frequency generator is 1.2 kW; the plasma gas flow is 16 mL/min; the flow rate of the atomized gas is 1.0 mL/min; the auxiliary gas flow is 0.2 mL/min; the lifting amount of the solution is 1.5 mL/min; the integration time is 2-5 s; the observation direction is axial; the observation height is 11 mm;
(2) reagent:
(2.1) gallium single element standard solution (1000 mug/mL, national iron and steel materials testing center iron and steel research institute);
(2.2) iron single element standard solution (10 mg/mL): is prepared by dissolving metal iron with the purity not less than 99.99 wt% by hydrochloric acid and nitric acid;
(2.3) hydrochloric acid,. rho.1.19 g/mL, CMOS grade;
(2.4) nitric acid,. rho.1.42 g/mL, CMOS grade;
(2.5) the test water is secondary water (the conductivity (25 ℃) is less than or equal to 0.10 mS/m);
(3) selection of analytical lines
Scanning and superposing a reagent blank, a matrix element solution, a coexistent element solution and a single element standard solution of an analysis element (the single element content in the single element standard solution is equal to the percentage content in a 0.1000g sample and respectively comprises 70 wt% of iron, 20 wt% of chromium, 10 wt% of nickel, 5 wt% of copper, 2 wt% of molybdenum and 0.1 wt% of gallium) at a gallium element spectral line, and selecting 417.206nm analytical lines with minimum spectral line interference as analytical spectral lines;
wherein, the reagent blank refers to an aqueous solution containing 1mL of nitric acid and 3mL of hydrochloric acid (the volume of the solution is 100 mL); the single element standard solution of the matrix element is 100mL of iron single element standard solution; the single element standard solution of the coexisting elements is 100mL of each of chromium, nickel, copper and molybdenum; the standard solution of elemental gallium is 100mL standard solution of elemental gallium.
The single element content is equivalent to the percentage content in a 0.1000g sample and is respectively as follows: in 100mL of a standard solution of iron monobasic, iron 70 wt% x 0.1000 g-0.07 g iron; 100mL of chromium single element standard solution, chromium 20 wt% x 0.1000 g-0.02 g chromium; 100mL of nickel single element standard solution, nickel 10 wt% x 0.1000g to 0.01g nickel; 100mL of copper single element standard solution, copper 5 wt% x 0.1000 g-0.005 g copper; in 100mL of molybdenum single element standard solution, molybdenum 2 wt% multiplied by 0.1000g to 0.002g molybdenum; in 100mL of gallium single element standard solution, gallium was 0.1 wt% x 0.1000g ═ 0.0001g gallium.
(4) Interference and cancellation of coexisting elements
The Ga417.206nm is mainly interfered by the spectral line and the matrix of the iron matrix, the interference of the iron matrix is eliminated by a matrix matching method, and the interference of the iron spectral line is deducted by taking a matrix blank as a standard working curve blank;
(5) measurement of
(5.1) preparation of test solution
Weighing 0.1000g of 304 antibacterial stainless steel sample to be detected in a 50mL beaker, adding 1mL of nitric acid and 3mL of hydrochloric acid, heating at the low temperature of 60 ℃ until the nitric acid and the hydrochloric acid are completely dissolved, taking down and cooling to room temperature, transferring the solution to a 100mL volumetric flask, diluting the solution to a scale with water, and uniformly mixing to form a test solution to be detected;
(5.2) preparation of Standard working Curve solution
Respectively transferring 7mL of the iron single element standard solution obtained in the step (2.2) into 5 100mL volumetric flasks, and respectively adding 1mL of nitric acid and 3mL of hydrochloric acid into each volumetric flask; then, adding gallium single element standard solutions with different amounts into the volumetric flasks respectively, diluting the solutions to a scale with water, and uniformly mixing the solutions; the percentage contents of gallium in the series of standard working curve solutions, which is equivalent to 0.1000g of a sample, are respectively as follows: 0 (matrix blank), 0.1 wt%, 0.5 wt%, 1 wt%, 5 wt%;
(5.3) measurement
Under the selected working condition of the instrument and the wavelength of the gallium analysis line, sequentially measuring the spectral intensity of gallium in the standard working curve solution in the step (5.2) according to the sequence of the concentration from low to high, repeating each solution for 2 times, and calculating the average value of the solution; and (3) drawing a standard working curve of gallium and calculating a correlation coefficient of the standard working curve by taking the average value of the spectral intensity minus the average value of the spectral intensity of the blank solution of the substrate as an ordinate and the percentage content of gallium as an abscissa (see figure 1). As can be seen from FIG. 1, the correlation coefficient r of the standard operating curve is not less than 0.999, and the linearity meets the requirement. Measuring the gallium element in the test solution in the step (5.1), repeating the measurement for 2 times, and calculating the average value of the gallium element; and subtracting the average value of the spectrum intensity of the matrix blank solution from the average value of the spectrum intensity of the sample to obtain the net spectrum intensity, and checking the percentage content of gallium in the sample from the standard working curve.
As shown in fig. 1, the standard working curve for gallium is y 20339.02x-52.91, x representing the mass percent (%) of gallium and y representing the relative intensity (cps).
(5.4) verification of precision and recovery
And (3) repeating the test solution in the step (5.1) for 6 times, and calculating the average value and the relative standard deviation (shown in table 1), wherein the relative standard deviation is less than 5 percent, and the precision is high. And (3) adding the gallium single element standard solution into the test solution obtained in the step (5.1), and calculating the standard addition recovery rate (see table 1) through a recovery test, wherein the recovery rate is between 98% and 101%, so that the requirements of production and scientific research are met.
TABLE 1 precision and recovery
(5.5) accuracy verification
The method of the present invention is used for measuring the gallium element in the synthetic test solution, and the result is shown in table 2. As can be seen from Table 2, the measurement results of the synthetic test solutions are consistent with the actual results, indicating that the method is highly accurate.
Wherein, the preparation process of the synthetic test solution is as follows: weighing 0.1000g of a common stainless steel sample without gallium into 2 50mL beakers, respectively adding a proper amount of gallium single element standard solution, wherein the content of the gallium single element standard solution is 0.1 wt% and 1.0 wt% of the content of the gallium single element standard solution in the 0.1000g sample, and preparing a test solution according to the step (5.1).
TABLE 2 determination of synthetic test solutions
| Numbering | Measured value wt% | True value wt% |
| 1 | 0.104 | 0.10 |
| 2 | 1.011 | 1.00 |
The embodiment result shows that the method uses aqua regia to dissolve the gallium-containing antibacterial stainless steel, eliminates the interference of an iron matrix by a matrix matching method, adopts a matrix blank as a standard working curve blank to eliminate the interference of an iron spectral line, and establishes an analysis and detection method for measuring the gallium content in the stainless steel by the inductively coupled plasma atomic emission spectrometry. The method is simple to operate, low in detection limit, high in precision, good in accuracy and wide in linear range, and can meet the detection requirement of gallium in novel antibacterial stainless steel.
Claims (3)
1. A method for measuring the content of gallium in antibacterial stainless steel is characterized by comprising the following steps:
(1) measuring on an inductively coupled plasma atomic emission spectrometer in an axial direction under the selected working parameters of the instrument and the wavelength of a gallium analysis line;
(2) reagent
(2.1) a gallium single element standard solution with the concentration of 1000 mug/mL;
(2.2) iron single element standard solution with concentration of 10 mg/mL: is prepared by dissolving metal iron with the purity not less than 99.99 wt% by hydrochloric acid and nitric acid;
(2.3) hydrochloric acid, [ rho ] 1.19g/mL, CMOS grade;
(2.4) nitric acid, [ rho ] 1.42g/mL, CMOS grade;
(2.5) the test water is secondary water, and the conductivity at 25 ℃ is less than or equal to 0.10 mS/m;
(3) selection of analytical lines
Selecting a gallium element spectral line of 417.206 nm;
(4) correction of disturbances in analysis lines
Eliminating interference of an iron matrix by a matrix matching method, and deducting interference of a ferrographic line by taking a matrix blank as a standard working curve blank;
(5) measurement of
(5.1) preparation of test solution
Weighing 0.1000g of a sample to be detected in a 50mL beaker, adding 1mL of nitric acid and 3mL of hydrochloric acid, heating at the low temperature of 60 ℃ until the nitric acid and the hydrochloric acid are completely dissolved, taking down and cooling to the room temperature, transferring the solution to a 100mL volumetric flask, diluting the solution to a scale with water, and uniformly mixing the solution to be detected;
(5.2) preparation of Standard working Curve solution
Firstly, respectively transferring 7mL of the iron single element standard solution obtained in the step (2.2) into 5 100mL volumetric flasks, and respectively adding 1mL of nitric acid and 3mL of hydrochloric acid into each volumetric flask; then, adding gallium single element standard solutions with different amounts into the volumetric flasks respectively, diluting the solutions to a scale with water, and uniformly mixing the solutions; the percentage contents of gallium in the series of standard working curve solutions, which is equivalent to 0.1000g of a sample, are respectively as follows: 0 (matrix blank), 0.1 wt%, 0.5 wt%, 1 wt%, 5 wt%;
(5.3) measurement
Under the selected working condition of the instrument and the wavelength of the gallium analysis line, sequentially measuring the spectral intensity of gallium in the standard working curve solution in the step (5.2) according to the sequence of the concentration from low to high, repeating each solution for 2 times, and calculating the average value of the solution; and (3) drawing a standard working curve of the gallium and calculating a correlation coefficient of the standard working curve by taking the average value of the spectral intensity minus the average value of the spectral intensity of the blank solution of the substrate as a vertical coordinate and the percentage content of the gallium as a horizontal coordinate, wherein the correlation coefficient is not less than 0.999.
2. The method for determining the content of gallium in the antibacterial stainless steel according to claim 1, characterized in that after the step (5.3), when the linearity of the working curve meets the requirement, the measurement of the gallium element in the test solution of the step (5.1) is carried out, the measurement is repeated for 2 times, and the average value is calculated; and subtracting the average value of the spectrum intensity of the matrix blank solution from the average value of the spectrum intensity of the sample to obtain the net spectrum intensity, and checking the percentage content of gallium in the sample from the standard working curve.
3. The method for determining the content of gallium in the antibacterial stainless steel according to claim 1, wherein in the step (1), the optimized working parameters of the inductively coupled plasma atomic emission spectrometer are as follows: the power of the high-frequency generator is 1.2 kW; the plasma gas flow is 16 mL/min; the flow rate of the atomized gas is 1.0 mL/min; the auxiliary gas flow is 0.2 mL/min; the lifting amount of the solution is 1.5 mL/min; the integration time is 2-5 s; the observation direction is axial; the height of observation was 11 mm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010078381A (en) * | 2008-09-24 | 2010-04-08 | Sumitomo Metal Mining Co Ltd | Method for high-precision analysis of metal elements by inductively-coupled plasma emission spectral analysis method |
| CN103940806A (en) * | 2014-04-10 | 2014-07-23 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for measuring gallium element in zinc oxide powder |
| CN106226288A (en) * | 2016-07-12 | 2016-12-14 | 广西壮族自治区分析测试研究中心 | The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target |
| CN108362684A (en) * | 2018-01-23 | 2018-08-03 | 中国航发北京航空材料研究院 | The analysis method of gallium element in a kind of measurement rafifinal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010078381A (en) * | 2008-09-24 | 2010-04-08 | Sumitomo Metal Mining Co Ltd | Method for high-precision analysis of metal elements by inductively-coupled plasma emission spectral analysis method |
| CN103940806A (en) * | 2014-04-10 | 2014-07-23 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for measuring gallium element in zinc oxide powder |
| CN106226288A (en) * | 2016-07-12 | 2016-12-14 | 广西壮族自治区分析测试研究中心 | The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target |
| CN108362684A (en) * | 2018-01-23 | 2018-08-03 | 中国航发北京航空材料研究院 | The analysis method of gallium element in a kind of measurement rafifinal |
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