CN110954383B - Method for measuring chromium content in vanadium-aluminum alloy - Google Patents
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Abstract
A method for measuring the chromium content in a vanadium-aluminum alloy comprises the following steps: firstly, the mass of the vanadium-aluminum alloy is m 1; secondly, crushing, powdering and aerobic combustion; thirdly, adding a nitric acid solution into the combustion product, and filtering to obtain a filtrate; fourthly, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the filtrate, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added; fifthly, adding a silver nitrate solution and an ammonium persulfate solution into the beaker, and reading the volume h1 of the solution; sixthly, preparing a titration reagent; seventhly, titrating the chromium-containing solution by using a titration reagent, and recording the titration volume h2 of the titration reagent; and eighthly, calculating the chromium content. According to the invention, the sample is crushed and calcined, so that chromium can be fully dissolved in nitric acid and hydrochloric acid solution, and carbide can be discharged at high temperature in the calcining process, so that the use amount of sulfuric acid is reduced, and the prepared reagent is used for color change determination, and the method is convenient and rapid.
Description
Technical Field
The invention relates to the field of chromium content detection, in particular to a method for determining chromium content in a vanadium-aluminum alloy.
Background
The vanadium-aluminum alloy is an important additive for producing titanium alloy, and the chemical component content of the main element and the content of chromium as an impurity element of the vanadium-aluminum alloy are required to be strictly controlled in the production process. The content of chromium not only affects the grade and grade of the aluminum-vanadium alloy, but also is easy to be segregated at the grain boundary of the titanium alloy after being taken as an additive, and the performance of the titanium alloy is seriously affected. Therefore, in the production of vanadium-aluminum alloy, the control of chromium element is very important, the existence of a large amount of vanadium in the vanadium-aluminum alloy interferes with the determination of chromium, the detection precision can reach below 0.3 percent by mainly analyzing and detecting through an ICP spectrometer, and the detection by using the method needs to purchase the ICP spectrometer, so the cost and the material consumption are high, and the detection is difficult to realize by common small and medium-sized enterprises. For the detection of the chromium content in the vanadium-aluminum alloy, on the premise of ensuring the accuracy of the detection result, particularly the detection of the low-chromium content in the vanadium-aluminum alloy, no good and economic chemical method can be circulated.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a method for measuring the chromium content in a vanadium-aluminum alloy without a complex instrument.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for measuring the chromium content in a vanadium-aluminum alloy comprises the following steps:
step one, taking a vanadium-aluminum alloy sample, weighing, and recording the mass of the vanadium-aluminum alloy sample as m1 (unit is gram);
step two, crushing and powdering the vanadium-aluminum alloy sample weighed in the step one, and placing the sample into a high-temperature combustor for aerobic combustion to obtain a combustion product;
step three, adding a nitric acid solution with the mass concentration of 10 percent, which is equivalent to 10 percent of the mass of the combustion product, into the combustion product obtained in the step two, and filtering to obtain a filtrate;
step four, adding the filtrate obtained in the step three into a beaker, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the beaker, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added;
step five, adding a silver nitrate solution and an ammonium persulfate solution into the beaker obtained in the step four, heating at a high temperature to promote trivalent chromium to be oxidized into hexavalent chromium to obtain a chromium-containing solution, and reading the volume h1 (unit is milliliter) of the solution;
the mass of silver nitrate in the silver nitrate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample, and the mass of ammonium persulfate in the ammonium persulfate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample;
the high-temperature heating temperature is 80-100 ℃, and the time is more than 20 minutes;
step six, weighing 20g of potassium permanganate and 10g of urea, adding the potassium permanganate and the urea into 200 ml of water, heating, stirring and dissolving, and pouring the solution into a beaker I; weighing 40g of phthalic anhydride and 5g of diphenylcarbodihydrazide, adding into the beaker I, diluting to 1 liter by using ethanol, and uniformly stirring to obtain a titration reagent;
step seven, taking 100ml of the chromium-containing solution obtained in the step five, titrating the chromium-containing solution by using the titration reagent obtained in the step six until the color is unchanged, and recording the titration volume h2 (unit is milliliter) of the titration reagent;
and step eight, calculating the chromium content.
Further, in the second step, the temperature of the aerobic combustion is 400-500 ℃, and the duration time is 2-4 minutes.
Further, in the step eight, the calculation is performed according to the following calculation formula:
W =（h1×h2）÷m1÷500。
according to the invention, the sample is crushed and calcined, so that chromium can be fully dissolved in nitric acid and hydrochloric acid solution, and carbide can be discharged at high temperature in the calcining process, so that the use amount of sulfuric acid is reduced, and the prepared reagent is used for color change determination, and the method is convenient and rapid. Is particularly suitable for measuring the chromium content in the vanadium-aluminum alloy with the chromium content of more than or equal to 0.01 percent.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The method for determining the chromium content in the vanadium-aluminum alloy comprises the following steps:
step one, taking a vanadium-aluminum alloy sample, weighing, and recording the mass m1 of the sample as 1000 g;
step two, crushing and powdering the vanadium-aluminum alloy sample weighed in the step one, and placing the sample into a high-temperature combustor for aerobic combustion to obtain a combustion product;
step three, adding a nitric acid solution with the mass concentration of 10 percent, which is equivalent to 10 percent of the mass of the combustion product, into the combustion product obtained in the step two, and filtering to obtain a filtrate;
step four, adding the filtrate obtained in the step three into a beaker, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the beaker, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added;
step five, adding a silver nitrate solution and an ammonium persulfate solution into the beaker obtained in the step four, heating at a high temperature to promote trivalent chromium to be oxidized into hexavalent chromium to obtain a chromium-containing solution, and reading the volume h1 of the solution to be 100 milliliters;
the mass of silver nitrate in the silver nitrate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample, and the mass of ammonium persulfate in the ammonium persulfate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample;
the high-temperature heating temperature is 90 ℃, and the time is 20 minutes;
step six, weighing 20g of potassium permanganate and 10g of urea, adding the potassium permanganate and the urea into 200 ml of water, heating, stirring and dissolving, and pouring the solution into a beaker I; weighing 40g of phthalic anhydride and 5g of diphenylcarbodihydrazide, adding into the beaker I, diluting to 1 liter by using ethanol, and uniformly stirring to obtain a titration reagent;
step seven, taking 100ml of the chromium-containing solution obtained in the step five, titrating the chromium-containing solution by using the titration reagent obtained in the step six until the color is unchanged, and recording the titration volume h2 of the titration reagent as 1 ml;
and step eight, calculating the chromium content.
In the second step, the aerobic combustion temperature is 400 ℃ and the duration time is 4 minutes.
And step eight, calculating according to the following calculation formula:
W =（h1×h2）÷m1÷500＝0.02%。
the content of chromium in the raw material of this example was analyzed and detected by an ICP spectrometer, and the detection result was 0.02%.
Example 2
The method for determining the chromium content in the vanadium-aluminum alloy comprises the following steps:
step one, taking a vanadium-aluminum alloy sample, weighing, and recording the mass m1 of the sample as 1000 g;
step two, crushing and powdering the vanadium-aluminum alloy sample weighed in the step one, and placing the sample into a high-temperature combustor for aerobic combustion to obtain a combustion product;
step three, adding a nitric acid solution with the mass concentration of 10 percent, which is equivalent to 10 percent of the mass of the combustion product, into the combustion product obtained in the step two, and filtering to obtain a filtrate;
step four, adding the filtrate obtained in the step three into a beaker, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the beaker, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added;
step five, adding a silver nitrate solution and an ammonium persulfate solution into the beaker obtained in the step four, heating at a high temperature to promote trivalent chromium to be oxidized into hexavalent chromium to obtain a chromium-containing solution, and reading the volume h1 of the solution to be 125 ml;
the mass of silver nitrate in the silver nitrate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample, and the mass of ammonium persulfate in the ammonium persulfate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample;
the high-temperature heating temperature is 80 ℃, and the time is 30 minutes;
step six, weighing 20g of potassium permanganate and 10g of urea, adding the potassium permanganate and the urea into 200 ml of water, heating, stirring and dissolving, and pouring the solution into a beaker I; weighing 40g of phthalic anhydride and 5g of diphenylcarbodihydrazide, adding into the beaker I, diluting to 1 liter by using ethanol, and uniformly stirring to obtain a titration reagent;
step seven, taking 100ml of the chromium-containing solution obtained in the step five, titrating the chromium-containing solution by using the titration reagent obtained in the step six until the color is unchanged, and recording the titration volume h2 of the titration reagent as 2 ml;
and step eight, calculating the chromium content.
In the second step, the aerobic combustion temperature is 450 ℃ and the duration time is 3 minutes.
And step eight, calculating according to the following calculation formula:
W =（h1×h2）÷m1÷500＝0.05％。
the content of chromium in the raw material of this example was analyzed and detected by an ICP spectrometer with a detection result of 0.05%.
Example 3
The method for determining the chromium content in the vanadium-aluminum alloy comprises the following steps:
step one, taking a vanadium-aluminum alloy sample, weighing, and recording the mass m1 of the sample as 1000 g;
step two, crushing and powdering the vanadium-aluminum alloy sample weighed in the step one, and placing the sample into a high-temperature combustor for aerobic combustion to obtain a combustion product;
step three, adding a nitric acid solution with the mass concentration of 10 percent, which is equivalent to 10 percent of the mass of the combustion product, into the combustion product obtained in the step two, and filtering to obtain a filtrate;
step four, adding the filtrate obtained in the step three into a beaker, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the beaker, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added;
step five, adding a silver nitrate solution and an ammonium persulfate solution into the beaker obtained in the step four, heating at a high temperature to promote trivalent chromium to be oxidized into hexavalent chromium to obtain a chromium-containing solution, and reading the volume h1 of the solution to be 250 milliliters;
the mass of silver nitrate in the silver nitrate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample, and the mass of ammonium persulfate in the ammonium persulfate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample;
the high-temperature heating temperature is 100 ℃, and the time is 20 minutes;
step six, weighing 20g of potassium permanganate and 10g of urea, adding the potassium permanganate and the urea into 200 ml of water, heating, stirring and dissolving, and pouring the solution into a beaker I; weighing 40g of phthalic anhydride and 5g of diphenylcarbodihydrazide, adding into the beaker I, diluting to 1 liter by using ethanol, and uniformly stirring to obtain a titration reagent;
step seven, taking 100ml of the chromium-containing solution obtained in the step five, titrating the chromium-containing solution by using the titration reagent obtained in the step six until the color is unchanged, and recording the titration volume h2 of the titration reagent as 2 ml;
and step eight, calculating the chromium content.
In the second step, the aerobic combustion temperature is 500 ℃ and the duration time is 2 minutes.
And step eight, calculating according to the following calculation formula:
W =（h1×h2）÷m1÷500＝0.10％。
the content of chromium in the raw material of this example was analyzed and detected by an ICP spectrometer, and the detection result was 0.10%.
Claims (2)
1. The method for measuring the chromium content in the vanadium-aluminum alloy is characterized by comprising the following steps of:
step one, taking a vanadium-aluminum alloy sample, weighing, and recording the mass of the vanadium-aluminum alloy sample as m 1;
step two, crushing and powdering the vanadium-aluminum alloy sample weighed in the step one, and placing the sample into a high-temperature combustor for aerobic combustion to obtain a combustion product;
step three, adding a nitric acid solution with the mass concentration of 10 percent, which is equivalent to 10 percent of the mass of the combustion product, into the combustion product obtained in the step two, and filtering to obtain a filtrate;
step four, adding the filtrate obtained in the step three into a beaker, dropwise adding a hydrochloric acid solution with the mass concentration of 20% into the beaker, and observing the color change in the beaker until the blue color in the beaker is not deepened after the hydrochloric acid solution is continuously dropwise added;
step five, adding a silver nitrate solution and an ammonium persulfate solution into the beaker obtained in the step four, heating at a high temperature to promote trivalent chromium to be oxidized into hexavalent chromium to obtain a chromium-containing solution, and reading the volume h1 of the solution;
the mass of silver nitrate in the silver nitrate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample, and the mass of ammonium persulfate in the ammonium persulfate solution is 1 percent of the mass of the raw material of the vanadium-aluminum alloy sample;
the high-temperature heating temperature is 80-100 ℃, and the time is more than 20 minutes;
step six, weighing 20g of potassium permanganate and 10g of urea, adding the potassium permanganate and the urea into 200 ml of water, heating, stirring and dissolving, and pouring the solution into a beaker I; weighing 40g of phthalic anhydride and 5g of diphenylcarbodihydrazide, adding into the beaker I, diluting to 1 liter by using ethanol, and uniformly stirring to obtain a titration reagent;
step seven, taking 100ml of the chromium-containing solution obtained in the step five, titrating the chromium-containing solution by using the titration reagent obtained in the step six until the color is unchanged, and recording the titration volume h2 of the titration reagent;
step eight, calculating the chromium content W;
and step eight, calculating according to the following calculation formula:
W =（h1×h2）÷m1÷500。
2. the method for determining the content of chromium in the vanadium-aluminum alloy as claimed in claim 1, wherein in the second step, the temperature of aerobic combustion is 400-500 ℃ and the duration is 2-4 minutes.
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