CN113155759A - Analytical test method for measuring silicon content in boron nitride by adopting spectrophotometry - Google Patents
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Abstract
The invention relates to an analysis and test method for measuring the silicon content in boron nitride by adopting a spectrophotometry, belonging to the technical field of chemical analysis of boron nitride. After the boron nitride sample is dissolved, silicon in the product is converted into soluble silicic acid, and the soluble silicic acid reacts with a color developing agent in an acid solution to generate a multi-heteropoly acid silicon-containing system. Reducing the multi-heteropoly acid silicon-containing system by using a reducing agent, wherein the absorbance of the obtained product is in direct proportion to the content of the multi-heteropoly acid silicon-containing system within a certain concentration range, namely, the absorbance can be measured by using a spectrophotometer, and then the silicon content can be calculated on a working curve. The method mainly solves the problem of measuring the silicon content in the boron nitride, has the advantages of high sensitivity, good selectivity, high accuracy, wide applicable concentration range, low analysis cost and simple and quick operation, and can be used as a conventional method for analyzing and testing the silicon content in the boron nitride.
Description
Technical Field
The invention relates to an analysis and test method for measuring the silicon content in boron nitride by adopting a spectrophotometry, belonging to the technical field of chemical analysis of boron nitride.
Background
Boron nitride is a crystal composed of nitrogen atoms and boron atoms. The chemical composition was 43.6% boron and 56.4% nitrogen with four different variants: hexagonal Boron Nitride (HBN), Rhombohedral Boron Nitride (RBN), Cubic Boron Nitride (CBN), and Wurtzite Boron Nitride (WBN). The boron nitride produced is generally of graphite type structure, commonly known as white graphite. The other is diamond type, and graphite type boron nitride can be converted into diamond type boron nitride under high temperature and high pressure, similar to the principle of converting graphite into diamond. Is a novel high-temperature resistant superhard material and is used for manufacturing drill bits, grinding tools and cutting tools. Boron nitride has wide application in the fields of aerospace, atomic reactor, metallurgy, chemical industry and the like.
At present, the method for measuring the impurity elements in the boron nitride mainly adopts a method for measuring the impurity elements in the boron nitride of GB/T34003-2017. the standard mainly provides the measurement of the impurity elements of lithium, sodium, calcium, magnesium, iron, zinc, copper, nickel, manganese, copper, titanium, strontium and cadmium in the boron nitride product by inductively coupled plasma atomic emission spectroscopy. The standard does not stipulate a method for measuring the silicon content in the boron nitride, the influence of the silicon content on the performance of the boron nitride material is increasingly remarkable along with the gradual progress of boron nitride research in recent years, and the accurate measurement of the silicon content in the boron nitride material has important significance on material research.
Disclosure of Invention
In order to solve the problem of measuring the silicon content in the boron nitride, the invention provides an analysis and test method for measuring the silicon content in the boron nitride by adopting a spectrophotometry, which has the characteristics of short flow, accurate result and easy operation.
The technical scheme for solving the technical problems comprises the following steps:
an analytical test method for measuring the silicon content in boron nitride by adopting a spectrophotometry method comprises the following steps:
(1) placing a boron nitride test sample in a nickel crucible, adding sodium hydroxide, uniformly mixing, covering with sodium peroxide, covering, placing in a preheated high-temperature furnace, heating and melting; simultaneously making a blank sample;
(2) putting the cooled nickel crucible and the sample into a beaker, adding water, and washing the crucible after the sample is completely leached;
(3) transferring the solution into a volumetric flask, and diluting with water until the total volume of the sample solution is V0Mixing, dry-filtering with medium-speed filter paper, and discarding the initial part of filtrate;
(4) adding part of the filtrate into a volumetric flask, dropwise adding a p-nitrophenol solution until the solution turns yellow, adjusting the solution to be colorless by using sulfuric acid, supplementing sulfuric acid, adding water, and uniformly mixing; adding the color developing agent solution under the condition of continuously shaking, uniformly mixing, and then standing;
(5) adding sulfuric acid, mixing, immediately adding a reducing agent solution, diluting with water, mixing, and standing;
(6) transferring part of the developed solution into a cuvette, taking blank solution of the sample as reference, and placing the cuvette at the position of 780-820nm (suitable for SiO) wavelength of a spectrophotometer2The amount is 0.10% -1.00%), or 600-700nm (suitable for SiO)2Measurement of>1.00 percent and less than or equal to 10.00 percent), and measuring the absorbance; the corresponding silica amount was calculated from the working curve.
In the step (1), the test sample is 0.1-0.5g, the addition amount of the sodium hydroxide is 0.5-5g, the use amount of the sodium peroxide is 0.1-1g, the preheating temperature of the high-temperature furnace is 200-.
In the step (4), the volume of the filtrate is divided into the total volume V of the sample solution01/60 to 1/10, the dripping amount of the paranitrophenol solution is 0.05 to 5mL, the concentration of the paranitrophenol solution is 0.1 to 10g/L, the solution turns yellow, the sulfuric acid is (1+1) sulfuric acid solution, and the adding amount of the sulfuric acid is 0.1 to 5 mL.
The color developing agent is selected from ammonium molybdate, potassium thiocyanate, methylene blue and the like which can form a multi-heteropoly acid silicon-containing system, wherein the ammonium molybdate is most commonly used.
The concentration of the developer solution is 1-200g/L, and the dosage of the developer solution can be 1-50mL, including but not limited to 1mL, 3mL, 5mL, 7mL, 10mL, 20mL, 30mL, 40mL, 50mL, etc.
Adding color developing agent, standing at 15-45 deg.C for 1-120min including but not limited to 1min, 3min, 5min, 7min, 10min, 20min, 30min, 50min, 60min, 80min, 100min, 120min, etc.
In the step (5), the sulfuric acid is a (1+1) sulfuric acid solution, and the addition amount of the sulfuric acid is 1-20 mL.
The choice of reducing agent includes, but is not limited to, ascorbic acid, ferrous sulfate, stannous chloride, hydroxylammonium hydrochloride, thiourea, and the like.
The concentration of the reducing agent solution is 5-100g/L, and the adding amount of the reducing agent solution is 1-50mL, including but not limited to 1mL, 3mL, 5mL, 7mL, 10mL, 20mL, 30mL, 40mL, 50mL and the like.
Adding reducing agent, reducing, standing at 15-45 deg.C for 1-120min including but not limited to 1min, 3min, 5min, 7min, 10min, 20min, 30min, 50min, 60min, 80min, 100min, 120min, etc.
Preferably, the method takes (1+1) sulfuric acid as a masking agent, ammonium molybdate as a color developing agent and ascorbic acid as a reducing agent to reduce the silicomolybdo xanthate heteropoly acid into a silicomolybdo blue complex.
In step (6), SiO in the boron nitride test sample2When the mass content of the compound is 0.10-1.00%, measuring the absorbance at a wavelength of 780-820nm by using a spectrophotometer; SiO in boron nitride test samples2In a mass content of>1.00 percent and less than or equal to 10.00 percent, and measuring the absorbance at the wavelength of 600-700nm by adopting a spectrophotometer.
The working curve is based on SiO in boron nitride test sample2The contents of (A) are plotted in two lines, each for SiO2A boron nitride test sample with a mass content of 0.10-1.00%, or SiO2In a mass content of>1.00 percent and less than or equal to 10.00 percent of boron nitride test samples.
The drawing method of the working curve for measuring the silicon content in the boron nitride comprises the following steps:
1) respectively transferring 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL of silicon dioxide standard solution into a volumetric flask, or respectively transferring 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of silicon dioxide standard solution into the volumetric flask, adding sulfuric acid, diluting with water, adding a color developing agent, uniformly mixing and standing;
2) adding sulfuric acid, mixing, immediately adding a reducing agent, diluting with water, mixing, and standing;
3) transferring a part of the color development solution into a cuvette, and measuring the absorbance of the color development solution at the wavelength of 780-820nm or 600-700nm of a spectrophotometer; and drawing a working curve by taking the amount of the silicon dioxide as an abscissa and the absorbance as an ordinate.
In step 1), the silica standard solution used to plot the working curve has a concentration of 1-200. mu.g/mL, including but not limited to 1. mu.g/mL, 3. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL, 30. mu.g/mL, 50. mu.g/mL, 100. mu.g/mL, 150. mu.g/mL, 200. mu.g/mL, and the like.
The sulfuric acid is (1+1) sulfuric acid solution, and the addition amount of the sulfuric acid is 0.5-20 mL.
The color developing agent is selected from ammonium molybdate, potassium thiocyanate, methylene blue and the like which can form a multi-heteropoly acid silicon-containing system, wherein the ammonium molybdate is most commonly used.
The concentration of the developer solution is 1-200g/L, and the dosage of the developer solution can be 1-50mL, including but not limited to 1mL, 3mL, 5mL, 7mL, 10mL, 20mL, 30mL, 40mL, 50mL, etc.
Adding color developing agent, standing at 15-45 deg.C for 1-120min including but not limited to 1min, 3min, 5min, 7min, 10min, 20min, 30min, 50min, 60min, 80min, 100min, 120min, etc.
In the step 2), the sulfuric acid is a (1+1) sulfuric acid solution, and the addition amount of the sulfuric acid is 1-20 mL.
The choice of reducing agent includes, but is not limited to, ascorbic acid, ferrous sulfate, stannous chloride, hydroxylammonium hydrochloride, thiourea, and the like.
The concentration of the reducing agent solution is 5-100g/L, and the adding amount of the reducing agent solution is 1-50mL, including but not limited to 1mL, 3mL, 5mL, 7mL, 10mL, 20mL, 30mL, 40mL, 50mL and the like.
Adding reducing agent, reducing, standing at 15-45 deg.C for 1-120min including but not limited to 1min, 3min, 5min, 7min, 10min, 20min, 30min, 50min, 60min, 80min, 100min, 120min, etc.
In step 3), for measuring SiO2The working curve of the boron nitride test sample with the mass content of 0.10-1.00 percent is measured at the wavelength of 780-minus 820nm of a spectrophotometer; for determining SiO2In a mass content of>1.00 percent and less than or equal to 10.00 percent, and measuring the absorbance at the wavelength of 600-700nm of a spectrophotometer.
Calculation of analysis results: the silica content in the sample was calculated from the working curve by the formula (1) and expressed as mass percent (%)
In the formula:
m1: from the working curveThe mass of silica is calculated in micrograms (μ g);
mblank space: calculating the mass of the silicon dioxide in micrograms (mug) in the blank sample from the working curve;
V0: total volume of test solution in milliliters (mL);
m0: the mass of the sample in grams (g);
V1: the volume of the test solution is divided in milliliters (mL).
The analysis results are shown to the two last decimal places.
In the invention, the adopted water is secondary distilled water with the purity of more than two times.
The above chemical reactions of the present invention mainly utilize: soluble silicic acid reacts with a color developing agent in an acid solution to generate a multi-heteropoly acid silicon-containing system. Reducing the multi-heteropoly acid silicon-containing system by using a reducing agent, wherein the absorbance of the obtained product is in direct proportion to the content of the multi-heteropoly acid silicon-containing system within a certain concentration range, namely, the absorbance can be measured by using a spectrophotometer, and then the silicon content can be calculated on a working curve.
The method adopts a spectrophotometry method for testing, has the advantages of high sensitivity, good selectivity, high accuracy, wide applicable concentration range, low analysis cost and simple and rapid operation, and can be used as a conventional method for analyzing and testing the silicon content in the boron nitride. The method is suitable for samples comprising boron nitride products such as Hexagonal Boron Nitride (HBN), Rhombohedral Boron Nitride (RBN), Cubic Boron Nitride (CBN), Wurtzite Boron Nitride (WBN) and the like.
Drawings
FIG. 1 is a working curve of example 1.
FIG. 2 is a working curve of example 2.
Detailed Description
The invention relates to an analysis and test method for measuring the silicon content in boron nitride by adopting a spectrophotometry, which comprises the following steps:
firstly, sample determination:
1. weighing 0.1-0.2g of test sample, placing in a 30mL nickel crucible, adding 2g of sodium hydroxide, mixing, covering with 0.5g of sodium peroxide, and covering. Placing in a high temperature furnace at 400 deg.C, heating to 800 deg.C, and melting for 30 min. Taking out and cooling slightly. Along with blank samples.
2. And (3) putting the cooled nickel crucible into a 300mL polytetrafluoroethylene beaker, adding 70mL of water, and washing out the crucible after complete leaching.
3. The solution was transferred to a 250mL plastic volumetric flask, diluted to the mark with water, mixed well, dry filtered through medium speed filter paper and the initial filtrate was discarded.
4. And (3) taking 10mL of filtrate, putting 0.2mL of p-nitrophenol into a 100mL plastic volumetric flask, dropwise adding until the solution turns yellow, adjusting the solution to be colorless by using (1+1) sulfuric acid, supplementing 0.5mL of (1+1) sulfuric acid, adding water until the volume is about 60mL, and uniformly mixing. 5mL of ammonium molybdate solution was added with constant shaking and mixed well. Standing at 25 deg.C for 20 min.
5. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
6. Transferring part of the developed solution into a 1cm cuvette, with blank solution of the sample as reference, at a wavelength of 810nm (suitable for SiO)2In an amount of 0.10% to 1.00%), or 660nm (suitable for SiO2Measured as>1.00%,. ltoreq.10.00%), and absorbance was measured. The corresponding silica amount was calculated from the working curve.
Drawing working curve
Is suitable for SiO2The content is 0.10 to 1.00 percent
1.0 mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL of silica standard solution (10. mu.g/mL) was transferred to a set of 100mL volumetric flasks, 0.5mL (1+1) of sulfuric acid was added, the mixture was diluted to 60mL with water, 5mL of ammonium molybdate solution was added, and the mixture was mixed well. Standing at 25 deg.C for 20 min.
2. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
3. A portion of the developed solution was transferred into a 1cm cuvette, and the absorbance thereof was measured at a wavelength of 810nm in a spectrophotometer. And drawing a working curve by taking the amount of the silicon dioxide as an abscissa and the absorbance as an ordinate.
(II) application to SiO2Measured as>1.00％、≤10.00％
1.0 mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL of silica standard solution (50. mu.g/mL) was transferred to a set of 100mL volumetric flasks, 0.5mL (1+1) of sulfuric acid was added, the mixture was diluted to 60mL with water, 5mL of ammonium molybdate solution was added, and the mixture was mixed well. Standing at 25 deg.C for 20 min.
2. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
3. A part of the developed solution was transferred into a 1cm cuvette, and the absorbance thereof was measured at a wavelength of 660nm in a spectrophotometer. And drawing a working curve by taking the amount of the silicon dioxide as an abscissa and the absorbance as an ordinate.
Thirdly, calculating the analysis result
The amount of silica is in mass fraction and the numerical value is expressed in%, calculated according to formula (1):
in the formula:
m1: the mass of silica in micrograms (μ g) was calculated from the working curve;
mblank space: calculating the mass of the silicon dioxide in micrograms (mug) in the blank sample from the working curve;
V0: total volume of test solution in milliliters (mL);
m0: the mass of the sample in grams (g);
V1: the volume of the test solution is divided in milliliters (mL).
The analysis results are shown to the two last decimal places.
The water is double distilled water with the purity above.
The present invention will be described in detail with reference to examples.
Example 1:
the analytical test method for measuring the silicon content in the boron nitride by adopting the spectrophotometry in the embodiment 1 of the invention adopts the following reagents:
sodium hydroxide is a premium grade pure solid powder.
The concentration of the p-nitrophenol is 1g/L aqueous solution.
(1+1) sulfuric acid is a solution of 98% concentrated sulfuric acid and water diluted in a volume ratio of 1: 1.
The ascorbic acid solution is L (+) -ascorbic acid aqueous solution, and the concentration is 50 g/L.
The color developing solution is ammonium molybdate solution (100 g/L).
Silicon standard solution (10. mu.g/mL).
The water is double distilled water with a purity of above, and at least double distilled water is adopted.
In this embodiment, the method for measuring the silicon content by using Hexagonal Boron Nitride (HBN) powder as a sample specifically includes the following steps:
firstly, drawing a working curve: is suitable for SiO2The content is 0.10 to 1.00 percent
1.0 mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL of silica standard solution (10. mu.g/mL) was transferred to a set of 100mL volumetric flasks, 0.5mL (1+1) of sulfuric acid was added, the mixture was diluted to 60mL with water, 5mL of ammonium molybdate solution was added, and the mixture was mixed well. Standing at 25 deg.C for 20 min.
2. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
3. A portion of the developed solution was transferred into a 1cm cuvette, and the absorbance thereof was measured at a wavelength of 810nm in a spectrophotometer. The amount of silica was plotted on the abscissa and the absorbance on the ordinate to obtain a working curve, as shown in FIG. 1.
Secondly, sample determination:
1. a0.2 g sample of boron nitride was weighed into a 30mL nickel crucible, 2g sodium hydroxide was added, mixed well, covered with 0.5g sodium peroxide, and covered. Placing in a high temperature furnace at 400 deg.C, heating to 800 deg.C, and melting for 30 min. Taking out and cooling slightly. Along with blank samples.
2. And (3) putting the cooled nickel crucible into a 300mL polytetrafluoroethylene beaker, adding 70mL of water, and washing out the crucible after complete leaching.
3. The solution was transferred to a 250mL plastic volumetric flask, diluted to the mark with water, mixed well, dry filtered through medium speed filter paper and the initial filtrate discarded.
4. And (3) putting 10mL of filtrate into a 100mL volumetric flask, dropwise adding 0.2mL of p-nitrophenol until the solution turns yellow, adjusting the solution to be colorless by using (1+1) sulfuric acid, supplementing 0.5mL of (1+1) sulfuric acid, adding water until the volume is about 60mL, and uniformly mixing. 5mL of ammonium molybdate solution was added with constant shaking and mixed well. Standing at 25 deg.C for 20 min.
5. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
6. A part of the developed solution was transferred into a 1cm cuvette, and the absorbance thereof was measured at a wavelength of 810nm in a spectrophotometer with reference to a blank test developed solution along with a sample. The corresponding amount of silica was checked from the working curve.
According to the formula (1), the mass content of the silicon dioxide in the tested sample is 0.21%.
Example 2:
this embodiment differs from embodiment 1 in that: in this example, the silicon content was measured using Cubic Boron Nitride (CBN) as a sample, and the other steps were the same as in example 1.
The reagents used were as follows:
sodium hydroxide is solid powder with high-grade purity;
the p-nitrophenol is an aqueous solution with the concentration of 1 g/L;
(1+1) the sulfuric acid is a solution of 98% concentrated sulfuric acid and water diluted according to the volume ratio of 1: 1;
the ascorbic acid solution is L (+) -ascorbic acid aqueous solution, and the concentration is 50 g/L.
The color developing solution is ammonium molybdate solution (100 g/L).
Silicon standard solution (50. mu.g/mL).
The water is double distilled water with a purity of above, and at least double distilled water is adopted.
The method specifically comprises the following steps:
firstly, drawing a working curve: is suitable for SiO2Measured as>1.00％、≤10.00％
1.0 mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL of silica standard solution (50. mu.g/mL) was transferred to a set of 100mL volumetric flasks, 0.5mL (1+1) of sulfuric acid was added, the mixture was diluted to 60mL with water, 5mL of ammonium molybdate solution was added, and the mixture was mixed well. Standing at 25 deg.C for 20 min.
2. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
3. A part of the developed solution was transferred into a 1cm cuvette, and the absorbance thereof was measured at a wavelength of 660nm in a spectrophotometer. The amount of silica was plotted on the abscissa and the absorbance on the ordinate to obtain a working curve, as shown in FIG. 2.
Secondly, sample determination:
1. a0.1 g sample of boron nitride was weighed into a 30mL nickel crucible, 2g sodium hydroxide was added, mixed well, covered with 0.5g sodium peroxide, and covered. Placing in a high temperature furnace at 400 deg.C, heating to 800 deg.C, and melting for 30 min. Taking out and cooling slightly. Along with blank samples.
2. The cooled nickel crucible was placed in a 300mL polyethylene beaker, 70mL water was added, and the crucible was washed out after complete leaching.
3. The solution was transferred to a 250mL volumetric flask, diluted to the mark with water, mixed well, dry filtered through medium speed filter paper and the initial filtrate discarded.
4. 10mL of filtrate is taken and put into a 100mL volumetric flask, 0.2mL of p-nitrophenol is dripped, the solution is adjusted to be colorless by (1+1) sulfuric acid, 0.5mL of (1+1) sulfuric acid is added, 20mL of water is added, and the mixture is mixed evenly. 5mL of ammonium molybdate solution was added with constant shaking and mixed well. Standing at 25 deg.C for 20 min.
5. Adding 10mL (1+1) sulfuric acid solution, mixing, immediately adding 3mL ascorbic acid solution, diluting with water to the scale, and mixing. Standing at 25 deg.C for 30 min.
6. A part of the developed solution was transferred to a 1cm cuvette, and the absorbance was measured at a wavelength of 660nm in a spectrophotometer with reference to a blank test developed solution along with a sample. The corresponding amount of silica was checked from the working curve.
According to the formula (1), the mass content of the silicon dioxide in the tested sample is 3.62%.
In example 1-2, the silicon content in boron nitride is measured by spectrophotometry, after a sample is dissolved by sodium hydroxide, the sample is cooled to a constant volume, a solution with a certain volume is taken, sulfuric acid (1+1) is used as a masking agent, ammonium molybdate is used as a color developing agent, ascorbic acid is used as a reducing agent to reduce silicomolybdo xanthate heteropoly acid into a silicomolybdo blue complex, the absorbance of the silicomolybdo xanthate heteropoly acid is measured by a spectrophotometer, and the silicon content is calculated on a working curve.
The color developing agent in the technical scheme of the invention is selected from ammonium molybdate, potassium thiocyanate, methylene blue and the like which can form the color developing agent of a multi-heteropoly acid silicon-containing system, wherein the ammonium molybdate is most commonly used. The amount of the developer includes, but is not limited to, 1mL, 3mL, 5mL, 7mL, 10mL, etc. The choice of reducing agent includes, but is not limited to, ascorbic acid, ferrous sulfate, stannous chloride, hydroxylammonium hydrochloride, thiourea, and the like. The time of standing after adding ammonium molybdate includes but is not limited to 10min, 20min, 30min, 50min, 60min and the like. Selection of the amount of ascorbic acid to use includes, but is not limited to, 1mL, 3mL, 5mL, 7mL, 10mL, and the like. The standing time after the ascorbic acid is added for reduction includes, but is not limited to, 10min, 20min, 30min, 50min, 60min and the like. The concentration of the silica standard solution used to plot the working curve includes, but is not limited to, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL, 30. mu.g/mL, 50. mu.g/mL, 100. mu.g/mL, and the like.
The method mainly solves the problem of measuring the silicon content in the boron nitride, has the advantages of high sensitivity, good selectivity, high accuracy, wide applicable concentration range, low analysis cost and simple and quick operation, and can be used as a conventional method for analyzing and testing the silicon content in the boron nitride.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. An analytical test method for measuring the silicon content in boron nitride by adopting a spectrophotometry method comprises the following steps:
(1) placing a boron nitride test sample in a nickel crucible, adding sodium hydroxide, uniformly mixing, covering with sodium peroxide, covering, placing in a preheated high-temperature furnace, heating and melting; simultaneously making a blank sample;
(2) putting the cooled nickel crucible and the sample into a beaker, adding water, and washing the crucible after the sample is completely leached;
(3) transferring the solution into a volumetric flask, and diluting with water until the total volume of the sample solution is V0Mixing, dry-filtering with medium-speed filter paper, and discarding the initial part of filtrate;
(4) adding part of the filtrate into a volumetric flask, dropwise adding a p-nitrophenol solution until the solution turns yellow, adjusting the solution to be colorless by using sulfuric acid, supplementing sulfuric acid, adding water, and uniformly mixing; adding the color developing agent solution under the condition of continuously shaking, uniformly mixing, and then standing;
(5) adding sulfuric acid, mixing, immediately adding a reducing agent solution, diluting with water, mixing, and standing;
(6) transferring part of the developed solution into a cuvette, taking the blank solution of the sample as a reference, and measuring the absorbance of the blank solution at the wavelength of 780-820nm or 600-700nm of a spectrophotometer; the corresponding silica amount was calculated from the working curve.
2. The analytical test method for measuring the silicon content in boron nitride by spectrophotometry as claimed in claim 1, wherein in the step (1), the test sample is 0.1-0.5g, the sodium hydroxide is 0.5-5g, the sodium peroxide is 0.1-1g, the preheating temperature of the high temperature furnace is 200-500 ℃, the temperature is raised to 600-1000 ℃, and the melting time is 10-150 min; in the step (4), the volume of the filtrate is divided into the total volume V of the sample solution01/60 to 1/10, the dripping amount of the paranitrophenol solution is 0.05 to 5mL, the concentration of the paranitrophenol solution is 0.1 to 10g/L, the solution turns yellow, the sulfuric acid is 1+1 sulfuric acid solution, and the adding amount of the sulfuric acid is 0.1 to 5 mL; in the step (5), the sulfuric acid is 1+1 sulfuric acid solution, and the sulfuric acid is addedThe dosage is 1-20 mL.
3. The analytical test method for measuring the content of silicon in boron nitride by spectrophotometry according to claim 1, wherein the method for drawing the working curve comprises the following steps:
1) respectively transferring 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL of silicon dioxide standard solution into a volumetric flask, or respectively transferring 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 6.00mL of silicon dioxide standard solution into the volumetric flask, adding sulfuric acid, diluting with water, adding a color developing agent, uniformly mixing and standing;
2) adding sulfuric acid, mixing, immediately adding a reducing agent, diluting with water, mixing, and standing;
3) transferring a part of the color development solution into a cuvette, and measuring the absorbance of the color development solution at the wavelength of 780-820nm or 600-700nm of a spectrophotometer; and drawing a working curve by taking the amount of the silicon dioxide as an abscissa and the absorbance as an ordinate.
4. The analytical test method for the spectrophotometric determination of the silicon content in boron nitride as claimed in claim 3, wherein the concentration of the standard solution of silicon dioxide is 1-200 μ g/mL.
5. The analytical test method for the spectrophotometric determination of the silicon content in boron nitride as claimed in claim 3, which is used for the determination of SiO2The working curve of the boron nitride test sample with the mass content of 0.10-1.00 percent is measured at the wavelength of 780-minus 820nm of a spectrophotometer; for determining SiO2In a mass content of>1.00 percent and less than or equal to 10.00 percent, and measuring the absorbance at the wavelength of 600-700nm of a spectrophotometer.
6. The analytical test method for the spectrophotometric determination of the silicon content of boron nitride according to claim 1 or 3, wherein the color-developing agent is ammonium molybdate, potassium thiocyanate or methylene blue.
7. The analytical test method for measuring the content of silicon in boron nitride by spectrophotometry according to claim 6, wherein the concentration of the color developing agent solution is 1-200g/L, and the dosage of the color developing agent solution can be 1-50 mL; adding color developing agent, standing at 15-45 deg.C for 1-120 min.
8. The analytical test method for determining the content of silicon in boron nitride by spectrophotometry according to claim 1 or 3, wherein the reducing agent is ascorbic acid, ferrous sulfate, stannous chloride, hydroxylammonium hydrochloride or thiourea.
9. The analytical test method for measuring the content of silicon in boron nitride by spectrophotometry according to claim 8, wherein the concentration of the reducing agent solution is 5-100g/L, and the addition amount of the reducing agent solution is 1-50 mL; adding reducing agent, reducing, standing at 15-45 deg.C for 1-120 min.
10. The analytical test method for the spectrophotometric determination of the silicon content in boron nitride as set forth in claim 1, wherein the silica content in the sample is calculated by the formula (1) based on the working curve, and the silica content is expressed as a mass percentage
In the formula:
m1: the mass of silica in micrograms (μ g) was calculated from the working curve;
mblank space: calculating the mass of the silicon dioxide in micrograms (mug) in the blank sample from the working curve;
V0: test solution totalityVolume in milliliters (mL);
m0: the mass of the sample in grams (g);
V1: the volume of the test solution is divided in milliliters (mL).
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