CN110687060B - Method for combined determination of phosphorus and silicon content in high-carbon ferrochrome and nitrided ferrochrome - Google Patents
Method for combined determination of phosphorus and silicon content in high-carbon ferrochrome and nitrided ferrochrome Download PDFInfo
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Abstract
The invention relates to the technical field of chemical analysis of steel and ferroalloy, and discloses a method for jointly determining the content of phosphorus and silicon in high-carbon ferrochrome and nitrided ferrochrome. The method comprises the following steps: s1, preparing mother liquor; s2, measuring phosphorus; s3, and measuring silicon. The method comprises the steps of firstly melting and decomposing a sample to be detected by using sodium peroxide, then dissolving the sample by using water, acidifying the sample by using perchloric acid, then adding hydrogen peroxide to reduce high-valence chromium in the sample to be detected into trivalent chromium, then completely decomposing redundant hydrogen peroxide by heating, and finally diluting the solution to a certain volume to obtain mother liquor. After the mother liquor is prepared, a part of the mother liquor is taken to measure the phosphorus in the sample to be measured by a bismuth phosphomolybdenum blue photometry, and a part of the mother liquor is taken to measure the silicon in the sample to be measured by a silicon molybdenum blue photometry. The method has the advantages of simple and convenient operation, high speed, accurate result and low cost, can simultaneously determine the contents of phosphorus and silicon in the sample, and does not generate toxic gas.
Description
Technical Field
The invention relates to the technical field of chemical analysis of steel and ferroalloy, in particular to a method for jointly measuring the contents of phosphorus and silicon in high-carbon ferrochrome and nitrided ferrochrome.
Background
The existing method for measuring the content of phosphorus and silicon in high-carbon ferrochrome and nitrided ferrochrome is to separately measure phosphorus and silicon. When the phosphorus content in high-carbon ferrochrome and ferrochrome nitride is measured, a sample is decomposed by sodium peroxide, then is soaked by water and is acidified by sulfuric acid, ferric iron is added, ammonia water is used for neutralization, phosphorus is precipitated and separated by ferric phosphate, and the high-valence chromium in the separated precipitate is volatilized by hydrochloric acid under the condition of exhausting perchloric acid smoke. When the content of silicon in high-carbon ferrochrome and ferrochrome nitride is measured by a silicomolybdenum blue photometry, a sample is decomposed by sodium peroxide, after being soaked by water and acidified by sulfuric acid, high-valence chromium is reduced to trivalent chromium by sodium sulfite, the trivalent iron is reduced to divalent iron, and excessive sulfurous acid is removed by heating and boiling.
At present, about 1500 to 2000 samples of high carbon ferrochrome and ferrochrome nitride are required to be detected in the company every year, and a method which is simple and convenient to operate, high in speed, accurate in result, low in cost and free of toxic gas is needed to be invented for measuring the content of phosphorus and silicon in the high carbon ferrochrome and the ferrochrome nitride.
Disclosure of Invention
The invention aims to overcome the problems that the methods for determining the contents of phosphorus and silicon in high-carbon ferrochrome and ferrochrome nitride in the prior art are silicon and phosphorus which are separately determined and toxic gas is generated in the determination process, and provides a method for jointly determining the contents of phosphorus and silicon in high-carbon ferrochrome and ferrochrome nitride.
In order to achieve the above object, the present invention provides a method for combined determination of phosphorus and silicon content in high carbon ferrochrome and ferrochrome nitride, which comprises the following steps:
s1, preparing mother liquor:
s11, mixing the sample to be tested with sodium peroxide, then covering the surface of the obtained mixture with sodium peroxide, melting, decomposing and cooling;
s12, dissolving the sample decomposed in the step S11 in water, adding perchloric acid for acidification, then adding hydrogen peroxide, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12, cooling, diluting with water, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, measuring two parts of the mother liquor obtained in the step S13, adding perchloric acid and ascorbic acid solution into one part of the mother liquor in sequence, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, ascorbic acid solution, bismuth salt solution, gum arabic-sodium thiosulfate mixed solution and ammonium molybdate solution into the other part in sequence, shaking up, diluting with water and shaking up to be used as color development liquid;
s22, taking the reference solution in the step S21 as a reference, selecting a wavelength, measuring the absorbance of the color development solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 5-6 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be detected according to the following formula (1):
wherein, W p Indicating that is to be measuredThe phosphorus content in the sample; m is 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, measuring two parts of the mother liquor obtained in the step S13, adding oxalic acid solution into one part of the mother liquor, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, an ammonium molybdate solution, an oxalic acid solution and an ammonium ferrous sulfate solution into the other part in sequence, shaking up, diluting with water, shaking up and standing to serve as a color development solution;
s32, taking the reference solution in the step S31 as a reference, selecting a wavelength, measuring the absorbance of the color development solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 5-6 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content and the corresponding absorbance in the standard sample;
s34, calculating the silicon content in the sample to be tested according to the following formula (2):
wherein, W Si Representing the content of silicon in a sample to be tested; m is 2 Represents the mass of silicon found on the operating curve in g; m represents the mass of the sample to be measured in g.
Preferably, in step S11, when the sample to be tested is mixed with sodium peroxide, the mass of the sample to be tested is 0.1-0.3g, and the mass of the sodium peroxide is 5-6 g.
Preferably, in step S11, the mass of sodium peroxide coated on the surface of the resultant mixture is 1-2 g.
Preferably, in step S11, the conditions of the melt decomposition are: the temperature is 700 ℃ and 720 ℃; the time is 10-12 minutes.
Preferably, in step S12, the decomposed sample is dissolved in 100-120mL of water.
Preferably, in step S12, perchloric acid is added in a volume of 29.5 to 30.5mL at a concentration of 70 to 72 mass%.
Preferably, in step S12, hydrogen peroxide is added in a volume of 9-11mL and at a concentration of 29.8-30.2 mass%.
Preferably, in step S13, the heating and boiling time is 3-5 minutes.
Preferably, after cooling, the solution is diluted to 199.8-200.2mL with water.
Preferably, in step S21, two portions of the mother liquor obtained in step S13 are measured, and the volume of the mother liquor is 19.8-20.2 mL.
Preferably, perchloric acid is added to the reference solution and the developing solution in a volume of 3.8 to 4.2mL, at a concentration of 70 to 72% by mass.
Preferably, in step S21, the ascorbic acid solution is added to the reference solution and the color developing solution in a volume of 2.8-3.2mL and at a concentration of 148-152 g/L.
Preferably, in step S21, in preparing the reference solution and the color developing solution, the two solutions are diluted to 49.8-50.2mL with water.
Preferably, in step S21, the bismuth salt solution is added to the color developing solution in a volume of 1.8-2.2mL and at a concentration of 49.5-50.5 g/L.
Preferably, in step S21, a gum arabic-sodium thiosulfate mixed solution is added to the color developing solution in a volume of 9.8 to 10.2mL, wherein the gum arabic solution has a concentration of 20 to 25g/L and the sodium thiosulfate solution has a concentration of 4.5 to 5.5 g/L.
Preferably, in step S21, the volume of the ammonium molybdate solution added to the color developing solution is 4.8-5.2mL, and the concentration is 49.5-50.5 g/L.
Preferably, in step S22, the selected wavelength is 690 nm.
Preferably, in step S31, two portions of the mother liquor obtained in step S13 are measured in volume of 4.8-5.2 mL.
Preferably, in step S31, the oxalic acid solution is added to the reference solution and the developing solution in a volume of 19.8-20.2mL and at a concentration of 49.5-50.5 g/L.
Preferably, in step S31, 9.8-10.2mL of perchloric acid with a concentration of 5+95 is added to the color developing solution.
Preferably, in step S31, the volume of the ammonium molybdate solution added to the color developing solution is 19.8-20.2mL, and the concentration is 24.5-25.5 g/L.
Preferably, in step S31, the volume of the ferrous ammonium sulfate solution added to the color developing solution is 4.8-5.2mL, and the concentration is 59.5-60.5 g/L.
Preferably, in step S31, in preparing the reference solution and the color developing solution, the two solutions are diluted to 99.8-100.2mL with water.
Preferably, in step S32, the selected wavelength is 730 nm.
The method comprises the steps of firstly melting and decomposing a sample to be detected by using sodium peroxide, then dissolving the sample by using water, acidifying the sample by using perchloric acid, then adding hydrogen peroxide to reduce high-valence chromium in the sample to be detected into trivalent chromium, then completely decomposing redundant hydrogen peroxide by heating, and finally diluting the solution to a certain volume to obtain a mother solution. After the mother liquor is prepared, a part of the mother liquor is taken to measure the phosphorus in the sample to be measured by a bismuth phosphomolybdenum blue photometry, and a part of the mother liquor is taken to measure the silicon in the sample to be measured by a silicon molybdenum blue photometry. The method has the advantages of simple and convenient operation, high speed, accurate result and low cost, can simultaneously determine the contents of phosphorus and silicon in the sample, and does not generate toxic gas.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for jointly measuring the content of phosphorus and silicon in high-carbon ferrochrome and nitrided ferrochrome, which is characterized by comprising the following steps of:
s1, preparing mother liquor:
s11, mixing the sample to be tested with sodium peroxide, then covering the surface of the obtained mixture with sodium peroxide, melting, decomposing and cooling;
s12, dissolving the sample decomposed in the step S11 in water, adding perchloric acid for acidification, then adding hydrogen peroxide, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12, cooling, diluting with water, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, measuring two parts of the mother liquor obtained in the step S13, adding perchloric acid and ascorbic acid solution into one part of the mother liquor in sequence, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, ascorbic acid solution, bismuth salt solution, gum arabic-sodium thiosulfate mixed solution and ammonium molybdate solution into the other part in sequence, shaking up, diluting with water, and shaking up to obtain color developing solution;
s22, taking the reference solution in the step S21 as a reference, selecting a wavelength, measuring the absorbance of the color development solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 5-6 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be detected according to the following formula (1):
wherein, W p Representing the content of phosphorus in a sample to be detected; m is a unit of 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, measuring two parts of the mother liquor obtained in the step S13, adding oxalic acid solution into one part of the mother liquor, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, an ammonium molybdate solution, an oxalic acid solution and an ammonium ferrous sulfate solution into the other part in sequence, shaking up, diluting with water, shaking up and standing to serve as a color development solution;
s32, taking the reference solution in the step S31 as a reference, selecting a wavelength, measuring the absorbance of the color development solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 5-6 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content in the standard sample and the corresponding absorbance;
s34, calculating the silicon content in the sample to be tested according to the following formula (2):
wherein, W Si Representing the content of silicon in a sample to be tested; m is a unit of 2 Represents the mass of silicon in g found from the operating curve; m represents the mass of the sample to be measured in g.
In the method, a sample to be detected is firstly molten and decomposed by sodium peroxide, dissolved by water and then acidified by perchloric acid, then the high valence chromium in the sample to be detected is reduced into trivalent chromium by hydrogen peroxide, and the solution is diluted to a certain volume after the hydrogen peroxide is completely decomposed by heating to obtain mother liquor; and then, taking a part of mother liquor to determine the phosphorus in the sample to be determined by a bismuth phosphomolybdenum blue photometry, and taking another part of mother liquor to determine the silicon in the sample to be determined by a silicon molybdenum blue photometry.
In the invention, the sample to be tested is a sample prepared according to GB/T20066 or a proper national standard; all the reagents are analytically pure reagents unless otherwise specified; the water is distilled water or deionized water, unless otherwise specified.
In the method of the present invention, in step S11, the prepared sample to be tested is first mixed with sodium peroxide and then melt-decomposed at a high temperature, and preferably, the sample to be tested and the sodium peroxide are mixed in a nickel crucible and melt-decomposed in a muffle furnace.
In step S11, when the sample to be tested is mixed with sodium peroxide, the mass of the sample to be tested is 0.1-0.3 g; specifically, the mass of the sample to be measured may be 0.1g, 0.15g, 0.2g, 0.25g, or 0.3 g; preferably, the mass of the sample to be measured is 0.2 g.
In step S11, when the sample to be tested is mixed with sodium peroxide, the mass of the sodium peroxide is 5-6 g; specifically, the mass of sodium peroxide may be 5g, 5.2g, 5.4g, 5.6g, 5.8g or 6 g; preferably, the mass of sodium peroxide is 5.5 g.
In the method of the present invention, in step S11, in order to better melt-decompose the solution to be measured, an appropriate amount of sodium peroxide may be coated on the surface of the mixture of the sample to be measured and the sodium peroxide. In step S11, the mass of sodium peroxide covered on the surface of the mixture is 1-2 g; specifically, the mass of sodium peroxide covered on the surface of the resulting mixture may be 1.2g, 1.4g, 1.6g, 1.8g, or 2 g; preferably, the mass of sodium peroxide coated on the surface of the resulting mixture is 1.5 g.
In the method of the present invention, in step S11, the conditions of the melt decomposition are: the temperature is 700 ℃ and 720 ℃, specifically, the temperature can be 700 ℃, 705 ℃, 710 ℃, 715 ℃ or 720 ℃, and preferably, the temperature is 700 ℃; the time is 10 to 12 minutes, specifically, the time may be 10 minutes, 10.5 minutes, 11 minutes, 11.5 minutes, or 12 minutes, and preferably, the time is 11 minutes.
In the method of the present invention, in step S12, after the sample to be measured is decomposed, it is necessary to dissolve the sample with an appropriate amount of water. In step S12, the decomposed sample is dissolved in 100-120mL of water; specifically, the decomposed sample may be dissolved in 100mL, 105mL, 110mL, 115mL, or 120mL of water; preferably, the decomposed sample is dissolved in 100mL of water.
In the method of the present invention, in step S12, after the sample to be tested is dissolved in water, it is necessary to acidify with an appropriate amount of acid, preferably perchloric acid.
In step S12, the perchloric acid is added in a volume of 29.5 to 30.5mL, specifically, the perchloric acid is added in a volume of 29.5mL, 30mL or 30.5mL, and preferably, the perchloric acid is added in a volume of 30 mL; in step S12, the perchloric acid is added at a concentration of 70 to 72 mass%, specifically, 70, 5, 71, 71.5, or 72 mass%, preferably 71 mass%.
In the method of the present invention, in order to convert the high valence chromium in the sample to be tested into trivalent chromium, an appropriate amount of hydrogen peroxide is added. In step S12, the volume of hydrogen peroxide added is 9-11mL, specifically, the volume of hydrogen peroxide added may be 9mL, 9.5mL, 10mL, 10.5mL or 11mL, preferably, the volume of hydrogen peroxide added is 10 mL; in step S12, the concentration of hydrogen peroxide added is 29.8 to 30.2 mass%, specifically, the concentration of hydrogen peroxide added may be 29.8 mass%, 29.9 mass%, 30 mass%, 30.1 mass%, or 30.2 mass%, and preferably, the concentration of hydrogen peroxide added is 30 mass%.
In the process of the present invention, the solution needs to be heated to boiling in order to decompose the remaining hydrogen peroxide. In step S13, the heating and boiling time is 3-5 minutes; specifically, the heating to boil may be for 3 minutes, 3.5 minutes, 4 minutes, 4.5 minutes, or 5 minutes; preferably, the heating and boiling time is 4 minutes.
And (4) cooling the heated solution, and diluting the cooled solution to a certain volume by using water to obtain mother liquor. In step S13, after cooling, diluting the solution to 199.8-200.2mL with water; specifically, after cooling, the solution may be diluted with water to 199.8mL, 199.9mL, 200mL, 200.1mL, or 200.2 mL; preferably, after cooling, the solution is diluted to 200mL with water.
In the method of the present invention, when determining the phosphorus content in a sample to be measured, two solutions are taken from the mother solution to prepare a reference solution and a developing solution, respectively, and the apparatus for preparing the reference solution and the developing solution can be a routine choice in the field, and preferably, the reference solution and the developing solution are prepared in volumetric flasks.
In step S21, two portions of the mother liquor obtained in step S13 are weighed, and the volume of the mother liquor is 19.8-20.2 mL; specifically, the volume of the mother liquor obtained in the two steps S13 may be 19.8mL, 19.9mL, 20mL, 20.1mL or 20.2 mL; preferably, the mother liquor obtained in step S13 is measured in two portions in a volume of 20 mL.
In step S21, the volume of perchloric acid added to the reference solution and the developing solution is 3.8 to 4.2mL, specifically, the volume of perchloric acid added to the reference solution and the developing solution may be 3.8mL, 3.9mL, 4.0mL, 4.1mL or 4.2mL, and preferably, the volume of perchloric acid added to the reference solution and the developing solution is 4 mL; in step S21, perchloric acid is added to the reference solution and the color developing solution at a concentration of 70 to 72 mass%, specifically, perchloric acid may be added to the reference solution and the color developing solution at a concentration of 70 mass%, 70.5 mass%, 71 mass%, 71.5 mass%, or 72 mass%, and preferably, perchloric acid is added to the reference solution and the color developing solution at a concentration of 71 mass%.
In step S21, the ascorbic acid solution is added to the reference solution and the developing solution in a volume of 2.8 to 3.2mL, specifically, the ascorbic acid solution may be added to the reference solution and the developing solution in a volume of 2.8mL, 2.9mL, 3.0mL, 3.1mL, or 3.2mL, and preferably, the ascorbic acid solution is added to the reference solution and the developing solution in a volume of 3.0 mL; in step S21, the ascorbic acid solution is added to the reference solution and the color developing solution at a concentration of 148-152g/L, specifically, the ascorbic acid solution is added to the reference solution and the color developing solution at a concentration of 148g/L, 149g/L, 150g/L, 151g/L or 152g/L, and preferably, the ascorbic acid solution is added to the reference solution and the color developing solution at a concentration of 150 g/L.
When the content of phosphorus in a sample to be measured is measured, when the reference solution and the color developing solution are prepared, after various reagents are added, the reference solution and the color developing solution are finally diluted to a certain volume for standby. In step S21, when preparing the reference solution and the developing solution, diluting the two solutions to 49.8-50.2mL by water; specifically, when preparing the reference solution and the color developing solution, the two solutions may be diluted with water to 49.8mL, 49.9mL, 50mL, 50.1mL, or 50.2 mL; preferably, when preparing the reference solution and the developing solution, the two solutions are diluted to 50mL with water.
In the method of the present invention, preferably, the bismuth salt solution is a bismuth nitrate solution. In step S21, adding a bismuth salt solution into the color developing solution in a volume of 1.8-2.2 mL; specifically, the volume of the bismuth salt solution added to the color developing solution may be 1.8mL, 1.9mL, 2.0mL, 2.1mL or 2.2 mL; preferably, the volume of the bismuth salt solution added to the color developing solution is 2 mL.
In step S21, bismuth salt solution is added into the color developing solution with the concentration of 49.5-50.5 g/L; specifically, the concentration of the bismuth salt solution added into the color development liquid can be 49.5g/L, 50g/L or 50.5 g/L; preferably, the bismuth salt solution is added to the color-developing solution at a concentration of 50 g/L.
In the method of the present invention, in step S21, the volume of the gum arabic-sodium thiosulfate mixed solution added to the color developing solution is 9.8 to 10.2mL, specifically, the volume of the gum arabic-sodium thiosulfate mixed solution added to the color developing solution may be 9.8mL, 10mL or 10.2mL, and preferably, the volume of the gum arabic-sodium thiosulfate mixed solution added to the color developing solution is 10 mL; wherein, in the mixed solution of the Arabic gum and the sodium thiosulfate, the concentration of the Arabic gum solution is 20-25g/L, specifically, the concentration of the Arabic gum solution can be 20g/L, 21g/L, 22g/L, 23g/L, 24g/L or 25g/L, and the concentration of the Arabic gum solution is preferably 22.5 g/L; in the gum arabic-sodium thiosulfate mixed solution, the concentration of the sodium thiosulfate solution is 4.5 to 5.5g/L, specifically, the concentration of the sodium thiosulfate solution can be 4.5g/L, 5g/L or 5.5g/L, and preferably, the concentration of the sodium thiosulfate solution is 5 g/L.
In the method of the invention, in step S21, the volume of the ammonium molybdate solution added into the color developing solution is 4.8-5.2 mL; specifically, the volume of the ammonium molybdate solution added into the color developing solution can be 4.8mL, 5.0mL or 5.2 mL; preferably, the volume of the ammonium molybdate solution added to the color developing solution is 5 mL.
In the method of the invention, in step S21, the concentration of ammonium molybdate solution added in the color developing solution is 49.5-50.5 g/L; specifically, the concentration of the ammonium molybdate solution added into the color developing solution can be 49.5g/L, 50g/L or 50.5 g/L; preferably, the concentration of the ammonium molybdate solution added into the color developing solution is 50 g/L.
In the method of the present invention, in determining the content of phosphorus in a test sample, after the reference solution and the developing solution are prepared, the reference solution and the developing solution are placed in a cuvette and the absorbances of the reference solution and the developing solution are measured at appropriate wavelengths, preferably, in order to improve the accuracy of the analysis result, the wavelength is selected to be 690nm in step S22.
In the process of preparing the color developing solution, after adding the ammonium molybdate solution, when the room temperature is less than 20 ℃, the prepared color developing solution needs to be placed in a constant-temperature water bath at 29-31 ℃ for 20 minutes, taken out, cooled to the room temperature and then measured for absorbance; when the room temperature is more than or equal to 20 ℃, the prepared developing solution is directly placed at the room temperature for 20 minutes, and then the absorbance of the developing solution is measured.
In the method of the present invention, when determining the content of silicon in a sample to be measured, two solutions are taken from the mother solution to prepare a reference solution and a developing solution, respectively, and the apparatus for preparing the reference solution and the developing solution can be a routine choice in the field, and preferably, the reference solution and the developing solution are prepared in a volumetric flask. When preparing the reference solution, only a proper amount of oxalic acid solution is added into the mother solution; when preparing the color developing solution, besides adding a proper amount of oxalic acid solution into the mother solution, proper amounts of perchloric acid, ammonium molybdate solution and ferrous ammonium sulfate solution are also added.
In the method, in step S31, two portions of the mother liquor obtained in step S13 are measured, and the volume of the mother liquor is 4.8-5.2 mL; specifically, the volume of the two portions of the mother liquor obtained in step S13 may be 4.8mL, 5mL or 5.2 mL; preferably, the volume of the mother liquor obtained in step S13 is taken in two portions of 5 mL.
In the method of the present invention, in step S31, the volume of the oxalic acid solution added to the reference solution and the developing solution is 19.8 to 20.2 mL; specifically, in step S31, the volume of the oxalic acid solution added to the reference solution and the developing solution may be 19.8mL, 20mL or 20.2 mL; preferably, the volume of the oxalic acid solution added to the reference solution and the developing solution is 20 mL.
In the method of the present invention, in step S31, the oxalic acid solution is added to the reference solution and the developing solution at a concentration of 49.5-50.5 g/L; specifically, the concentration of the oxalic acid solution added in the reference solution and the developing solution can be 49.5g/L, 50g/L or 50.5 g/L; preferably, the concentration of the oxalic acid solution added in the reference solution and the developing solution is 50 g/L.
In the method of the invention, in step S31, 9.8-10.2mL of perchloric acid with the concentration of 5+95 is added into the color developing solution; specifically, 9.8mL, 10mL or 10.2mL of 5+ 95-concentration perchloric acid can be added to the color developing solution; preferably, 10mL of perchloric acid having a concentration of 5+95 is added to the color former.
In the method of the invention, in step S31, the volume of the ammonium molybdate solution added into the color developing solution is 19.8-20.2 mL; specifically, the volume of the ammonium molybdate solution added into the color developing solution can be 19.8mL, 20mL or 20.2 mL; preferably, the volume of the ammonium molybdate solution added to the color developing solution is 20 mL.
In the method of the invention, in step S31, the concentration of the ammonium molybdate solution added into the color developing solution is 24.5-25.5 g/L; specifically, the concentration of the ammonium molybdate solution added into the color developing solution can be 24.5g/L, 25g/L or 25.5 g/L; preferably, the concentration of the ammonium molybdate solution added into the color developing solution is 25 g/L.
In the process of determining the silicon content in a sample to be detected, after adding an ammonium molybdate solution when preparing a color developing solution, when the room temperature is less than 20 ℃, the solution needs to be placed in a constant-temperature water bath at 29-31 ℃ for 10-15 minutes, taken out, cooled to the room temperature, and then added with other reagents; when the room temperature is more than or equal to 20 ℃, the solution needs to be placed at the room temperature for 10 to 15 minutes and then other reagents are added.
In the method of the invention, in step S31, the volume of the ferrous ammonium sulfate solution added into the color development liquid is 4.8-5.2 mL; specifically, the volume of the ammonium ferrous sulfate solution added into the color development solution can be 4.8mL, 5mL or 5.2 mL; preferably, the volume of the ferrous ammonium sulfate solution added to the color developing solution is 5 mL.
In the method of the invention, in step S31, the concentration of the ferrous ammonium sulfate solution added into the color development solution is 59.5-60.5 g/L; specifically, the concentration of the ammonium ferrous sulfate solution added into the color development liquid can be 59.5g/L, 60g/L or 60.5 g/L; preferably, the concentration of the ferrous ammonium sulfate solution added into the color developing solution is 60 g/L.
In the process of measuring the silicon content in the sample to be measured, when the reference solution and the developing solution are prepared, after various reagents are added, the reference solution and the developing solution are finally diluted to a certain volume for standby.
In the method of the present invention, in step S31, in preparing the reference solution and the developing solution, the two solutions are diluted to 99.8-100.2mL with water; specifically, when preparing the reference solution and the developing solution, the two solutions may be diluted to 99.8mL, 100mL or 100.2mL with water; preferably, when preparing the reference solution and the developing solution, the solutions are diluted to 100mL with water.
In the process of determining the silicon content in the sample to be measured, after the preparation of the reference solution and the developing solution is completed, the reference solution and the developing solution are placed in a cuvette to measure the absorbance of the reference solution and the developing solution at a suitable wavelength, preferably, in step S32, in order to improve the accuracy of the analysis result, the selected wavelength is 730 nm.
The method comprises the steps of firstly melting and decomposing a sample to be detected by using sodium peroxide, then dissolving the sample by using water, acidifying the sample by using perchloric acid, then adding hydrogen peroxide to reduce high-valence chromium in the sample to be detected into trivalent chromium, then completely decomposing redundant hydrogen peroxide by heating, and finally diluting the solution to a certain volume to obtain a mother solution. After the mother liquor is prepared, a part of the mother liquor is taken to measure the phosphorus in the sample to be measured by a bismuth phosphomolybdenum blue photometry, and a part of the mother liquor is taken to measure the silicon in the sample to be measured by a silicon molybdenum blue photometry. The method has the advantages of simple and convenient operation, high speed, accurate result and low cost, can simultaneously determine the contents of phosphorus and silicon in the sample, and does not generate toxic gas.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
The 1# -5# samples to be tested used in the embodiment of the invention are standard samples which are 1# (carbon ferrochrome, BH0310-3), 2# (high-carbon ferrochrome, YSBC28622-2010), 3# (high-nitrogen ferrochrome, GSB03-2196-2008), 4# (carbon ferrochrome, BH0310-4) and 5# (high-carbon ferrochrome, GBW (E) 010256). In the embodiment, the 1# to 5# samples to be tested are prepared according to GB/T20066 before being prepared into mother liquor.
Example 1
S1, preparing mother liquor:
s11, mixing 0.2g of No. 1 sample to be tested with 5.5g of sodium peroxide in a nickel crucible, then covering 1.5g of sodium peroxide on the surface of the obtained mixture, putting the mixture in a muffle furnace, melting and decomposing the mixture for 11 minutes at 700 ℃, and cooling the mixture;
s12, dissolving the sample to be tested decomposed in the step S11 with 100mL of water, adding 30mL of perchloric acid with the concentration of 71 mass percent for acidification, then adding 10mL of hydrogen peroxide with the concentration of 30 mass percent, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12 for 4 minutes, cooling, diluting with water to 200mL, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, weighing two 20mL portions of the mother liquor obtained in the step S13 into two 50mL volumetric flasks, adding 4mL of perchloric acid with the concentration of 71 mass percent and 3mL of ascorbic acid solution with the concentration of 150g/L into one portion of the mother liquor in sequence, shaking up, diluting with water to a scale, shaking up to be used as reference liquor; adding 4mL of perchloric acid with the concentration of 71 mass percent, 3mL of ascorbic acid solution with the concentration of 150g/L, 2mL of bismuth nitrate solution with the concentration of 50g/L, 10mL of a mixed solution of gum arabic and sodium thiosulfate and an ammonium molybdate solution into the other part in sequence, wherein the concentration of the gum arabic solution is 22.5g/L, and the concentration of the sodium thiosulfate solution is 5g/L, shaking up, diluting with water to a scale, shaking up and using as a color developing solution;
s22, taking the reference solution in the step S21 as a reference, selecting 690nm as a wavelength, measuring the absorbance of the color development solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 6 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be measured according to the following formula (1):
wherein, W p Representing the content of phosphorus in a sample to be detected; m is a unit of 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, weighing two 5mL portions of the mother liquor obtained in the step S13 into two 100mL volumetric flasks, adding 20mL of oxalic acid solution with the concentration of 50g/L into one portion of the mother liquor, shaking up, diluting with water to a scale, and shaking up to be used as reference liquor; adding 10mL of 5+ 95-concentration perchloric acid, 20mL of 25g/L ammonium molybdate solution, 20mL of 50g/L oxalic acid solution and 5mL of 60g/L ferrous ammonium sulfate solution into the other part in sequence, shaking up, diluting with water to a scale, shaking up, standing for 20 minutes to serve as a color developing solution;
s32, taking the reference solution in the step S31 as a reference, selecting 730nm as a wavelength, measuring the absorbance of the developing solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 5 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content and the corresponding absorbance in the standard sample;
s34, calculating the silicon content in the sample to be measured according to the following formula (2):
wherein, W Si Representing the content of silicon in a sample to be tested; m is a unit of 2 Represents the mass of silicon found on the operating curve in g; m represents the mass of the sample to be measured in g.
Example 2
S1, preparing mother liquor:
s11, mixing 0.2g of 2# sample to be tested with 5g of sodium peroxide in a nickel crucible, then covering 2g of sodium peroxide on the surface of the obtained mixture, placing the mixture in a muffle furnace, melting and decomposing the mixture for 10 minutes at 720 ℃, and cooling the mixture;
s12, dissolving the sample to be tested decomposed in the step S11 with 110mL of water, adding 30.5mL of perchloric acid with the concentration of 70 mass percent for acidification, then adding 11mL of hydrogen peroxide with the concentration of 30.2 mass percent, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12 for 3.5 minutes, cooling, diluting with water to 200mL, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, weighing two 20mL portions of the mother liquor obtained in the step S13 into two 50mL volumetric flasks, adding 4.2mL of perchloric acid with the concentration of 70% by mass and 2.8mL of ascorbic acid solution with the concentration of 151g/L into one portion of the mother liquor in sequence, shaking up, diluting with water to a scale, and shaking up to be used as reference liquor; adding 4.2mL of perchloric acid with the concentration of 70 mass%, 2.8mL of ascorbic acid solution with the concentration of 151g/L, 2.2mL of bismuth nitrate solution with the concentration of 49.5g/L, 10.2mL of a mixed solution of Arabic gum and sodium thiosulfate and an ammonium molybdate solution into the other part in sequence, wherein the concentration of the Arabic gum solution is 22.5g/L, the concentration of the sodium thiosulfate solution is 4.8g/L, shaking up, diluting with water to a scale, shaking up to obtain a color developing solution;
s22, taking the reference solution in the step S21 as a reference, selecting 690nm as a wavelength, measuring the absorbance of the developing solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 5 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be measured according to the following formula (1):
wherein the content of the first and second substances,W p representing the content of phosphorus in a sample to be detected; m is 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, weighing two 5mL portions of mother liquor obtained in the step S13 into two 100mL volumetric flasks, adding 19.8mL of oxalic acid solution with the concentration of 50.5g/L into one portion of the mother liquor, shaking up, diluting with water to a scale, shaking up, and taking the diluted solution as a reference solution; adding 10.2mL of 5+95 perchloric acid with concentration, 19.8mL of 25.5g/L ammonium molybdate solution, 19.8mL of 50.5g/L oxalic acid solution and 5.2mL of 59.5g/L ammonium ferrous sulfate solution into the other part in sequence, shaking up, diluting with water to a scale, shaking up, standing for 20 minutes to serve as color development liquid;
s32, taking the reference solution in the step S31 as a reference, selecting 730nm as a wavelength, measuring the absorbance of the color development solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 6 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content and the corresponding absorbance in the standard sample;
s34, calculating the silicon content in the sample to be tested according to the following formula (2):
wherein, W Si Representing the silicon content in the sample to be tested; m is 2 Represents the mass of silicon found on the operating curve in g; m represents the mass of the sample to be measured in g.
Example 3
S1, preparing mother liquor:
s11, mixing 0.2g of No. 3 sample to be tested with 6g of sodium peroxide in a nickel crucible, then covering 1g of sodium peroxide on the surface of the obtained mixture, placing the mixture in a muffle furnace, melting and decomposing the mixture for 12 minutes at 705 ℃, and cooling the mixture;
s12, dissolving the sample to be tested decomposed in the step S11 with 120mL of water, adding 30mL of perchloric acid with the concentration of 72 mass percent for acidification, then adding 9mL of hydrogen peroxide with the concentration of 30.2 mass percent, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12 for 4.5 minutes, cooling, diluting with water to 200mL, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, weighing two 20mL portions of mother liquor obtained in the step S13 into two 50mL volumetric flasks, adding 3.8mL of perchloric acid with the concentration of 72% by mass and 3.2mL of ascorbic acid solution with the concentration of 149g/L into one portion of the mother liquor in sequence, shaking up, diluting with water to a scale, and shaking up to be used as reference liquor; adding 3.8mL of 72 mass% perchloric acid, 3.2mL of 149g/L ascorbic acid solution, 1.8mL of 50.5g/L bismuth nitrate solution, 9.8mL of a mixed solution of gum arabic and sodium thiosulfate and an ammonium molybdate solution into the other part in sequence, wherein the concentration of the gum arabic solution is 20g/L, and the concentration of the sodium thiosulfate solution is 5.5g/L, shaking up, diluting with water to a scale, shaking up to obtain a color developing solution;
s22, taking the reference solution in the step S21 as a reference, selecting 690nm as a wavelength, measuring the absorbance of the color development solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 6 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be detected according to the following formula (1):
wherein, W p Representing the content of phosphorus in a sample to be detected; m is 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, weighing two 5mL portions of mother liquor obtained in the step S13 into two 100mL volumetric flasks, adding 20.2mL of oxalic acid solution with the concentration of 49.5g/L into one portion, shaking up, diluting with water to a scale, shaking up, and taking the diluted solution as a reference solution; adding 9.8mL of perchloric acid with the concentration of 5+95, 20.2mL of ammonium molybdate solution with the concentration of 24.8g/L, 20.2mL of oxalic acid solution with the concentration of 49.5g/L and 4.8mL of ferrous ammonium sulfate solution with the concentration of 60.5g/L into the other part in sequence, shaking up, diluting with water to scale, shaking up, standing for 20 minutes to serve as a color development liquid;
s32, taking the reference solution in the step S31 as a reference, selecting 730nm as a wavelength, measuring the absorbance of the color development solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 6 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content in the standard sample and the corresponding absorbance;
s34, calculating the silicon content in the sample to be measured according to the following formula (2):
wherein, W Si Representing the silicon content in the sample to be tested; m is 2 Represents the mass of silicon in g found from the operating curve; m represents the mass of the sample to be measured in g.
Example 4
The procedure was as described in example 1, except that the phosphorus and silicon contents of the test sample No. 4 were measured.
Example 5
The procedure was followed as described in example 1 except that the phosphorus and silicon contents of the test sample No. 5 were measured.
The results of measuring phosphorus and silicon in test samples # 1 to # 5 in examples 1 to 5 are shown in tables 1 and 2, respectively.
TABLE 1
TABLE 2
As can be seen from the results in tables 1 and 2, the method for determining the content of phosphorus and silicon in the high-carbon ferrochrome and the high-carbon ferrochrome nitride ferrochrome has the advantages that the difference between the determination result and the corresponding standard value is less than the national standard allowable difference, and the determination result is accurate.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (19)
1. A method for jointly measuring the content of phosphorus and silicon in high-carbon ferrochrome and nitrided ferrochrome is characterized by comprising the following steps:
s1, preparing mother liquor:
s11, mixing the sample to be tested with sodium peroxide, then covering the surface of the obtained mixture with sodium peroxide, melting, decomposing and cooling;
s12, dissolving the sample decomposed in the step S11 in water, adding perchloric acid for acidification, then adding hydrogen peroxide, and stirring for reaction;
s13, heating and boiling the solution obtained in the step S12, cooling, diluting with water, and uniformly mixing to obtain mother liquor;
s2, determination of phosphorus:
s21, measuring two parts of the mother liquor obtained in the step S13, adding perchloric acid and ascorbic acid solution into one part of the mother liquor in sequence, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, ascorbic acid solution, bismuth salt solution, gum arabic-sodium thiosulfate mixed solution and ammonium molybdate solution into the other part in sequence, shaking up, diluting with water and shaking up to be used as color development liquid;
s22, taking the reference solution in the step S21 as a reference, selecting the wavelength to be 690nm, measuring the absorbance of the developing solution in the step S21 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s23, taking 5-6 parts of standard sample, operating according to the steps S11-S22, and drawing a working curve of the phosphorus content and the corresponding absorbance in the standard sample;
s24, calculating the phosphorus content in the sample to be detected according to the following formula (1):
Wherein, W p Representing the content of phosphorus in a sample to be detected; m is 1 Represents the mass of phosphorus found on the working curve in g; m represents the mass of the sample to be measured, and the unit is g;
s3, measurement of silicon:
s31, measuring two parts of the mother liquor obtained in the step S13, adding oxalic acid solution into one part of the mother liquor, shaking up, diluting with water, and shaking up to be used as reference liquor; adding perchloric acid, an ammonium molybdate solution, an oxalic acid solution and an ammonium ferrous sulfate solution into the other part in sequence, shaking up, diluting with water, shaking up and standing to serve as a color development solution;
s32, taking the reference solution in the step S31 as a reference, selecting the wavelength of 730nm, measuring the absorbance of the color development solution in the step S31 on a spectrophotometer by using a cuvette, and recording the absorbance data;
s33, taking 5-6 parts of standard sample, operating according to the steps S11-S13 and S31-S33, and drawing a working curve of the silicon content and the corresponding absorbance in the standard sample;
s34, calculating the silicon content in the sample to be tested according to the following formula (2):
wherein, W Si Representing the content of silicon in a sample to be tested; m is 2 Represents the mass of silicon in g found from the operating curve; m representsMeasuring the mass of the sample, wherein the unit is g;
in step S11, when the sample to be tested is mixed with sodium peroxide, the mass of the sample to be tested is 0.1-0.3g, the mass of the sodium peroxide is 5-6g, and the mass of the sodium peroxide covered on the surface of the mixture is 1-2 g.
2. The method according to claim 1, wherein in step S11, the conditions of the melt decomposition are: the temperature is 700-720 ℃; the time is 10-12 minutes.
3. The method as claimed in claim 1, wherein in step S12, the decomposed sample is dissolved in 120mL of water with a volume of 100-.
4. The method according to claim 1, wherein in step S12, perchloric acid is added in a volume of 29.5 to 30.5mL at a concentration of 70 to 72% by mass.
5. The method according to claim 1, wherein in step S12, hydrogen peroxide is added in a volume of 9 to 11mL in a concentration of 29.8 to 30.2 mass%.
6. The method as claimed in claim 1, wherein the heating and boiling time is 3-5 minutes in step S13.
7. The method of claim 1, wherein in step S13, after cooling, the solution is diluted to 199.8-200.2mL with water.
8. The method of claim 1, wherein in step S21, two portions of the mother liquor obtained in step S13 are measured out, and the volume of the mother liquor is 19.8-20.2 mL.
9. The method according to claim 1, wherein in step S21, perchloric acid is added to the reference solution and the color developing solution in a volume of 3.8 to 4.2mL, and at a concentration of 70 to 72% by mass.
10. The method as claimed in claim 1, wherein in step S21, the ascorbic acid solution is added to the reference solution and the color developing solution in a volume of 2.8-3.2mL and at a concentration of 148-152 g/L.
11. The method according to claim 1, wherein in step S21, in preparing the reference solution and the color developing solution, the two solutions are diluted with water to 49.8-50.2 mL.
12. The method according to claim 1, wherein in step S21, the bismuth salt solution is added to the color-developing solution in a volume of 1.8 to 2.2mL and at a concentration of 49.5 to 50.5 g/L.
13. The method according to claim 1, wherein in step S21, a gum arabic-sodium thiosulfate mixed solution is added to the color developing solution in a volume of 9.8 to 10.2mL, wherein the gum arabic solution has a concentration of 20 to 25g/L, and the sodium thiosulfate solution has a concentration of 4.5 to 5.5 g/L.
14. The method according to claim 1, wherein in step S21, the ammonium molybdate solution is added to the color developing solution in a volume of 4.8 to 5.2mL and at a concentration of 49.5 to 50.5 g/L.
15. The method of claim 1, wherein in step S31, two portions of the mother liquor obtained in step S13 are measured out, and the volume of the mother liquor is 4.8-5.2 mL.
16. The method according to claim 1, wherein the oxalic acid solution is added to the reference solution and the developing solution in a volume of 19.8 to 20.2mL and at a concentration of 49.5 to 50.5g/L in step S31.
17. The method according to claim 1, wherein in step S31, the volume of the ammonium molybdate solution added to the color developing solution is 19.8 to 20.2mL, and the concentration is 24.5 to 25.5 g/L.
18. The method according to claim 1, wherein in step S31, the volume of the ferrous ammonium sulfate solution added to the color developing solution is 4.8-5.2mL, and the concentration is 59.5-60.5 g/L.
19. The method according to claim 1, wherein in step S31, in preparing the reference solution and the color developing solution, the two solutions are diluted to 99.8-100.2mL with water.
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