CN112578076A - Chemical detection method for vanadium element in aluminum-vanadium alloy - Google Patents
Chemical detection method for vanadium element in aluminum-vanadium alloy Download PDFInfo
- Publication number
- CN112578076A CN112578076A CN201910934415.9A CN201910934415A CN112578076A CN 112578076 A CN112578076 A CN 112578076A CN 201910934415 A CN201910934415 A CN 201910934415A CN 112578076 A CN112578076 A CN 112578076A
- Authority
- CN
- China
- Prior art keywords
- solution
- vanadium
- concentration
- aluminum
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a chemical detection method for vanadium element in aluminum-vanadium alloy, which comprises the following steps: sampling and pretreating the aluminum-vanadium alloy: weighing a sample, placing the sample in a container, adding a hydrochloric acid solution, a nitric acid solution and water, heating for dissolving, adding a sulfuric acid solution after the sample is completely dissolved, continuously heating a phosphoric acid solution, dropwise adding nitric acid to destroy carbides, smoking until the distance between sulfur and phosphoric acid smoke is about 1-2 cm from the liquid level of the solution, taking down the mixture for cooling slightly, adding water, and cooling to room temperature; calibrating an ammonium ferrous sulfate solution; adding potassium permanganate solution into the obtained solution, adding urea and sodium nitrite solution, using N-phenyl-o-aminobenzoic acid as indicator, and using ammonium ferrous sulfate solution to make titration to end point. The invention has the advantages of reasonable design, advanced technology, compact and smooth process, good detection efficiency and precision, detection cost reduction, good performance price ratio, avoidance of heavy pollution metal and products thereof, reduction of environmental pollution risk, energy conservation and emission reduction, safety, reliability, practicability and high efficiency.
Description
Technical Field
The invention relates to a process method for detecting metal chemical elements in the industries of metallurgy, machinery and the like, in particular to a method for detecting vanadium elements in aluminum-vanadium alloy.
Background
Vanadium, chemical element symbol V, silver white metal, belonging to group VB of the periodic table of elements, atomic number 23, atomic weight 50.9414. Vanadium has a high melting point and is often combined with niobium, tantalum, tungsten, molybdenum and is known as a refractory metal. The alloy has the characteristics of ductility, hard quality, no magnetism and the like, has the performance of resisting hydrochloric acid and sulfuric acid at intervals, is stable in compact metal vanadium at room temperature, does not react with air, water and alkali, can resist dilute acid, and has better gas resistance, salt resistance and water corrosion resistance than most stainless steels. Therefore, the vanadium metal is known as monosodium glutamate in modern industry, is widely applied to the fields of steel, chemical industry, aerospace and the like, can improve the performances of wear resistance, strength, hardness, ductility and the like of steel by adding vanadium into the steel, can improve the strength of the steel by 10-20 percent by adding 0.1 percent of vanadium, reduces the structural weight by 15-25 percent, and reduces the cost by 8-10 percent.
The aluminum-vanadium alloy is silver gray metal luster block-shaped in appearance, and the metal luster is enhanced, the hardness is increased and the oxygen content is increased along with the increase of the vanadium content in the alloy. The aluminum-vanadium alloy is a high-grade alloy material widely used in the field of aerospace, has high hardness, elasticity, seawater resistance and lightness, is commonly used for manufacturing a water glider of a water aerocraft box, and has very wide market application prospect along with the development of metal material industry.
The Al-V alloy is used as intermediate alloy, mainly as intermediate alloy for producing Ti alloy and high-temp. alloy, and as element additive for some special alloys (especially for vacuum smelting). 3 grades of 50%, 65% and 85% according to the vanadium content, and the balance of aluminum. The vanadium-aluminum alloy has low gas content, and other impurities such as Fe, Si, C, B and the like need to meet the requirements of the titanium alloy. The vanadium pentoxide for producing the titanium-aluminum alloy is high-purity vanadium pentoxide for purifying industrial products again to ensure that the impurity content reaches a specified range, and the aluminum is high-purity aluminum.
For the special steel metallurgy field, the aluminum vanadium alloy is a main additive for producing titanium alloy Ti-6 Al-4V. Therefore, the content of each chemical element in the aluminum vanadium alloy is ensured to meet the technical requirements, and the key point of special metallurgy preparation production is provided. As for the chemical detection process, the method provides quick, effective and correct inspection data, which is a key step for ensuring the Ti-6Al-4V titanium alloy product.
At present, the state of vanadium element in the aluminum-vanadium alloy has no mandatory and recommended detection standard, and all enterprises generally analyze and detect the chemical content of the metal vanadium according to the detection standard GB/T8704.5-94 'potentiometric titration method for determining the vanadium content'. The main process is characterized in that: dissolving a sample by using nitric acid and sulfuric acid, oxidizing vanadium (IV) into vanadium (V) by using slightly excessive potassium permanganate, decomposing excessive potassium permanganate by using sodium nitrite, and decomposing excessive sodium nitrite by using urea; the method is characterized in that potentiometric titration is carried out by using ammonium ferrous sulfate standard solution to determine the vanadium content, and the detection model (reaction formula) is as follows:
the method can meet the chemical analysis and detection of the content of metal vanadium in the aluminum-vanadium alloy to a certain extent, but because the ferrovanadium and the aluminum-vanadium alloy are not the same matrix after all, certain difference exists, and the ferrovanadium and the aluminum-vanadium alloy cannot be completely executed according to the GB/T8704.5-94 standard, so that the existing chemical detection process method has certain defects, namely:
1) the processing process of the sample is not applicable, the nitric acid and the sulfuric acid are adopted for dissolving the sample for the ferrovanadium, but the two acids cannot completely process the sample of the aluminum vanadium alloy, so that the distortion of chemical analysis data is caused.
2) The potentiometric titrator needs to be calibrated and metered regularly, certain metering cost is generated, the chemical detection cost is increased, and the mass production organization is not facilitated;
3) the environment protection pressure is higher, because the calomel electrode used by the potentiometric titrator contains metal mercury in the material, the metal mercury and the products thereof belong to heavy pollution metals, and certain environmental pollution risks exist in the production, storage and use processes.
In conclusion, on the premise that the aluminum vanadium alloy does not have the national and industry related professional detection standard, corresponding process technology optimization and improvement are carried out on the processes of sample pretreatment, titration and the like according to the characteristics of the aluminum vanadium alloy on the basis of fully utilizing the GB/T8704.5-94 standard, the precision and the speed of chemical detection of metal vanadium are guaranteed, the production cost is reduced on the basis of meeting the technical requirements of special alloy smelting, and the detection quality and the detection efficiency are improved.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a chemical detection method for vanadium element in aluminum-vanadium alloy.
The invention has the technical scheme that the chemical detection method for vanadium element in the aluminum-vanadium alloy comprises the following steps:
1) sampling and pretreating the aluminum-vanadium alloy: weighing a sample, placing the sample in a container, adding a hydrochloric acid solution, a nitric acid solution and water, heating for dissolving, adding a sulfuric acid solution after the sample is completely dissolved, continuously heating a phosphoric acid solution, dropwise adding nitric acid to destroy carbides, smoking until the distance between sulfur and phosphoric acid smoke is about 1-2 cm from the liquid level of the solution, taking down the mixture for cooling slightly, adding water, and cooling to room temperature;
the mass concentration of the hydrochloric acid is more than 20%; the mass concentration of the nitric acid is more than 40%; the mass concentration of the sulfuric acid is more than 70%; the mass concentration of the phosphoric acid solution is more than 70%; the upper limit is the highest concentration available on the market;
the ratio of the sample to the hydrochloric acid solution is (0.1-0.5:5-10) g/mL, the ratio of the sample to the nitric acid solution is (0.1-0.5:5-10) g/mL, the ratio of the sample to the sulfuric acid solution is (0.1-0.5:8-20) g/mL, and the ratio of the sample to the phosphoric acid solution is (0.1-0.5:5-10) g/mL;
2) calibrating an ammonium ferrous sulfate solution;
3) titration operation: dripping potassium permanganate solution into the solution obtained in the step 1) until stable red is generated, then dripping 1-2 drops of the potassium permanganate solution, uniformly mixing, standing, adding solid urea or urea solution, then dripping sodium nitrite solution to reduce excessive potassium permanganate until the solution is bright yellow, then dripping sodium nitrite solution, uniformly mixing and standing; dripping N-phenyl-o-aminobenzoic acid indicator, immediately titrating with ferrous ammonium sulfate standard solution until the color of the solution is changed from cherry red to bright green;
V3: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator;
m: weight (g) of sample.
The solid urea or urea solution acts to decompose excess sodium nitrite, acting as a matrix for the solution. Preferably, solid urea is added. Preferably, the solid urea is added in an amount of 0.5-2 g. The reinforcing body is convenient for use.
Preferably, the ratio of the sample to the hydrochloric acid solution is (0.1-0.5:5-10) g/mL; the ratio of the sample to the nitric acid solution is (0.1-0.5:5-10) g/mL; the ratio of the sample to the sulfuric acid solution is (0.1-0.5:10-12) g/mL; the ratio of the sample to the phosphoric acid solution was (0.1-0.5:5-8) g/mL. More preferably, the ratio of the sample to the phosphoric acid solution is (0.1-0.5:5-6) g/mL.
According to the chemical detection method for vanadium element in aluminum-vanadium alloy, preferably, in the step 1), the mass percentage concentration of the hydrochloric acid solution is 36-38%, the mass percentage concentration of the nitric acid solution is 65-68%, the mass percentage concentration of the sulfuric acid solution is 95-98%, and the mass percentage concentration of the phosphoric acid solution is more than 85%. The concentrations of the hydrochloric acid solution, the nitric acid solution, the sulfuric acid solution and the phosphoric acid solution are the most concentrated reagents sold in the market.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, preferably, the step 2) of calibrating the ferrous ammonium sulfate solution is as follows: absorbing potassium dichromate standard solution into a reaction container, adding sulfuric acid solution and phosphoric acid solution, adding water, cooling, dropwise adding N-phenyl anthranilic acid indicator, titrating with to-be-calibrated ammonium ferrous sulfate solution until the solution turns from rose red to bright green, and recording the volume of the consumed ammonium ferrous sulfate solution as V1; the corrected value for the N-phenylanthranilic acid indicator is V2;
the concentration of the ferrous ammonium sulfate solution is calculated according to the following formula:
c: concentration (mol/L) of potassium dichromate standard solution;
v: removing the volume (mL) of the potassium dichromate standard solution;
V1: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, further, the potassium dichromate standard solution in the step 2) is 0.05-0.15 mol/l; the dosage of the potassium dichromate standard solution is 8-15 mL; the volume ratio of the sulfuric acid solution to the potassium dichromate standard solution is 1: 0.8-1.2; the volume ratio of the phosphoric acid solution to the potassium dichromate standard solution is 1: 0.4-0.6.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, further, in the step 2), the mass concentration of the sulfuric acid is more than 70%; the mass concentration of the phosphoric acid solution is more than 70%; the upper limit is the highest concentration available on the market.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, further, in the step 2), 20-100 mL of water is added. According to the capacity of the container, the solution has proper volume, and the titration is convenient.
According to the chemical detection method for vanadium element in aluminum-vanadium alloy, the correction of the N-phenyl-substituted anthranilic acid indicator means that after the volume of the consumed ammonium ferrous sulfate solution obtained for the first time is V1, potassium dichromate standard solution with the same concentration and volume is added, the ammonium ferrous sulfate solution to be calibrated is continuously titrated until the solution is changed from rose red to bright green, and the difference value between the volume of the ammonium ferrous sulfate solution used for the second time and V1 is V2. V2 corresponds to the volume of ferrous ammonium sulfate solution consumed by the indicator.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, the concentration of the potassium permanganate solution in the step 3) is preferably 1.0-3.5%;
preferably, the concentration of the sodium nitrite solution in the step 3) is 0.5-2%.
Preferably, the standing time of step (3) is 1 to 10 minutes. The addition of the sodium nitrite solution is less than 10 drops. More preferably, the sodium nitrite solution is 1-2 drops.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, the concentration of the N-phenyl anthranilic acid indicator is preferably 0.1-0.3%.
According to the chemical detection method for vanadium element in the aluminum-vanadium alloy, the concentration of the ammonium ferrous sulfate standard solution in the step 3) is preferably 0.03-0.10 mol/L.
The invention is particularly suitable for the chemical detection process of vanadium element in the aluminum-vanadium alloy in the early stage of large-scale steel smelting production.
The invention designs a chemical detection method for vanadium element in aluminum-vanadium alloy, which is a process improvement aiming at the current chemical analysis detection mode of vanadium element in aluminum-vanadium alloy. The method comprises the steps of sample sampling and pretreatment → titration operation (process) → chemical analysis and the like, wherein hydrochloric acid, nitric acid, phosphoric acid and sulfuric acid are adopted for dissolving in the sample pretreatment process, vanadium is oxidized into pentavalent vanadium through potassium permanganate at room temperature, excessive potassium permanganate is adopted for reduction through sodium nitrite in the presence of urea, phenyl anthranilic acid is used as an indicator, and ammonium ferrous sulfate standard solution is used for titration. The invention has the advantages of reasonable design, advanced technology, compact and smooth process, good detection efficiency and precision, detection cost reduction, good performance price ratio, avoidance of heavy pollution metal and products thereof, reduction of environmental pollution risk, energy conservation and emission reduction, safety, reliability, practicability and high efficiency. The method effectively meets the requirement of chemical classification detection operation in the vacuum smelting production of the aluminum-vanadium alloy, is an original technology in the chemical analysis field of the aluminum-vanadium alloy produced by special metallurgy in China, has strong universality, improves the chemical analysis mode of the content of metal vanadium in the aluminum-vanadium alloy in the industry, has certain reference and application values, and has wide market prospect.
The invention has the beneficial effects that:
1. the design is reasonable, the technology is advanced, the process is compact and smooth, the detection efficiency is improved by more than 2 times, and the method is an original technology in the chemical analysis field of the special metallurgy production of the aluminum-vanadium alloy in China;
2. three acid solutions of phosphoric acid, sulfuric acid and nitric acid are adopted in the sample pretreatment process, vanadium is oxidized into pentavalent vanadium by potassium permanganate under the condition of room temperature, and then sodium nitrite is used for reduction, phenyl-substituted anthranilic acid is used as an indicator, and ammonium ferrous sulfate standard solution is used for titration;
3. the detection efficiency and precision are good, the detection cost is reduced, the performance price is good, particularly heavy pollution metal and products thereof are avoided, the environmental pollution risk is reduced, the energy is saved, the emission is reduced, and the method is safe, reliable, practical and efficient;
4. the operation method is quick, simple and convenient, is easy to master by operators, meets the requirement of daily chemical detection precision, is suitable for the field of large-scale production, and effectively meets the requirement of chemical classification detection operation in the vacuum smelting production of the aluminum-vanadium alloy;
5. the method has strong universality, improves the chemical analysis mode of the vanadium content in the aluminum-vanadium alloy in the industry, has certain reference and application values, and has wide market prospect.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
Example 1
The invention provides a chemical detection method for vanadium element in aluminum-vanadium alloy, which is implemented by a detection center and is a process improvement aiming at the chemical analysis detection mode of vanadium element in the aluminum-vanadium alloy. The method comprises the steps of sample sampling and pretreatment → a titration process → chemical analysis and the like (see figure 1), wherein hydrochloric acid, nitric acid, phosphoric acid and sulfuric acid are adopted for dissolving in the sample pretreatment process, vanadium is oxidized into pentavalent vanadium by potassium permanganate under the room temperature condition, excessive potassium permanganate is adopted for reduction by using sodium nitrite under the existence of urea, phenyl-substituted anthranilic acid is used as an indicator, and ammonium ferrous sulfate standard solution is used for titration. The main process method comprises the following steps:
1) sampling and pretreating the aluminum-vanadium alloy: weighing 0.2000g of sample, placing the sample in a 500mL conical flask, adding 5mL of hydrochloric acid, 5mL of nitric acid and 10mL of water, heating for dissolving, adding 10mL of sulfuric acid and 5mL of phosphoric acid after the sample is completely dissolved, continuing heating, dropwise adding nitric acid to destroy carbide, smoking until the bottom of the flask is about half inch empty, taking down the flask for cooling slightly, adding 100mL of water, and cooling to room temperature.
2) Titration operation (procedure): dropwise adding a potassium permanganate solution (2.5%) until stable red is generated, dropwise adding 1-2 drops of the potassium permanganate solution (2.5%), uniformly mixing, standing for 4-5 minutes, adding 1 g of urea (solid), dropwise adding a sodium nitrite solution (1%) to reduce excessive potassium permanganate until the solution is bright yellow, dropwise adding 1-2 drops of the sodium nitrite solution (1%), uniformly mixing, and standing for 1 minute. 3 drops of N-phenylanthranilic acid indicator (0.2%) were added and immediately titrated with a ferrous ammonium sulfate standard solution (0.05mol/L) to the end point where the color of the solution turned from cherry red to bright green.
3) The chemical analysis process of the vanadium content of the metal comprises the following steps:
a. preparing operation: reagents, metering devices, glassware preparation, etc.
b. The pretreatment process of the aluminum-vanadium alloy sample comprises the following steps:
sampling and pretreating the aluminum-vanadium alloy: weighing 0.2000g of sample, placing the sample in a 500mL conical flask, adding 5mL of hydrochloric acid, 5mL of nitric acid and 10mL of water, heating for dissolving, adding 10mL of sulfuric acid and 5mL of phosphoric acid after the sample is completely dissolved, continuing heating, dropwise adding the nitric acid to destroy carbide, smoking until the distance between sulfur and phosphoric acid smoke and the bottom liquid level of the flask is about 1-2 cm, taking down the flask for cooling slightly, adding 100mL of water, and cooling to room temperature.
c. Calibration of ferrous ammonium sulfate and correction of indicator:
suck 10mL ofAdding 0.10mol/l potassium dichromate standard solution into a 300mL conical flask, adding 10mL sulfuric acid, 5mL phosphoric acid and 50mL water, cooling, adding 3 drops of indicator, titrating with the ammonium ferrous sulfate solution to be calibrated until the solution changes from rose red to bright green, and recording the volume of the consumed ammonium ferrous sulfate solution as V1Adding 10ml of 0.10N potassium dichromate standard solution, continuously titrating with the ferrous ammonium sulfate solution to be calibrated until the solution changes from rose red to bright green, wherein the difference between the volume of the ferrous ammonium sulfate solution consumed by the ferrous ammonium sulfate solution and the volume of the ferrous ammonium sulfate solution consumed by the ferrous ammonium sulfate solution is the corrected value V of 3 drops of the N-phenyl-o-aminobenzoic acid indicator2。
The concentration of the ferrous ammonium sulfate solution is calculated according to the following formula:
c: concentration (mol/L) of potassium dichromate standard solution;
v: removing the volume (mL) of the potassium dichromate standard solution;
V1: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator.
d. And (3) detection:
titration operation (procedure): dropwise adding a potassium permanganate solution (2.5%) until stable red is generated, dropwise adding 1-2 drops of the potassium permanganate solution (2.5%), uniformly mixing, standing for 4-5 minutes, adding 1 g of urea (solid), dropwise adding a sodium nitrite solution (1%) to reduce excessive potassium permanganate until the solution is bright yellow, dropwise adding 1-2 drops of the sodium nitrite solution (1%), uniformly mixing, and standing for 1 minute. 3 drops of N-phenylanthranilic acid indicator (0.2%) were added and immediately titrated with a ferrous ammonium sulfate standard solution (0.05mol/L) to the end point where the color of the solution turned from cherry red to bright green.
e. And (4) calculating a result:
V3: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator;
m: weight (g) of sample.
V1 ═ 19.08, V2 ═ 0.02, V3 ═ 39.55, and calculated, the content of V is given by the formula: 52.82 percent.
f. Finishing: data acquisition and registration, instrument and tool closing, chemical reagent recovery, glassware cleaning and the like.
According to the process (parameter) model content, the precise, rapid, safe and pollution-free chemical operation of the vanadium content in the aluminum-vanadium alloy for vacuum smelting can be completed.
Example 2:
the pretreatment process comprises the following steps: weighing 0.1000g of sample, placing the sample in a 500mL conical flask, adding 2.5mL of hydrochloric acid, 2.5mL of nitric acid and 10mL of water, heating for dissolving, adding 10mL of sulfuric acid and 5mL of phosphoric acid after the sample is completely dissolved, continuing heating, dropwise adding the nitric acid to destroy carbide, smoking until the distance between sulfur and phosphoric acid is about 1-2 cm from the bottom liquid level of the flask, taking down the flask for cooling slightly, adding 100mL of water, and cooling to room temperature.
Titration operation (procedure): dropwise adding a potassium permanganate solution (2.5%) until stable red is generated, dropwise adding 1-2 drops of the potassium permanganate solution (2.5%), uniformly mixing, standing for 4-5 minutes, adding 1 g of urea (solid), dropwise adding a sodium nitrite solution (1%) to reduce excessive potassium permanganate until the solution is bright yellow, dropwise adding 1-2 drops of the sodium nitrite solution (1%), uniformly mixing, and standing for 1 minute. 3 drops of N-phenylanthranilic acid indicator (0.2%) were added and immediately titrated with a ferrous ammonium sulfate standard solution (0.03mol/L) until the color of the solution turned from cherry red to bright green. The rest is the same as example 1.
V1-35.05, V2-0.02, V3-31.80, calculated to give V content by the formula: 46.22 percent.
The chemical detection method for vanadium element in the aluminum-vanadium alloy adopts three acid liquids of phosphoric acid, sulfuric acid and nitric acid to pretreat a sample, oxidizes vanadium into pentavalent vanadium by potassium permanganate at room temperature, adopts excessive potassium permanganate to reduce by sodium nitrite in the presence of urea, adopts phenyl substituted anthranilic acid as an indicator, and titrates by ammonium ferrous sulfate standard solution. The device has the advantages of reasonable design, advanced technology, compact and smooth process, good detection efficiency and precision, detection cost reduction, good performance price ratio, avoidance of heavy pollution of metals and products thereof, reduction of environmental pollution risks, energy conservation and emission reduction, safety, reliability, practicability and high efficiency, improvement of the detection efficiency by more than 2 times, effective satisfaction of the requirement of chemical composition detection operation in the vacuum smelting production of the aluminum-vanadium alloy, and capability of creating economic benefits of more than 100 ten thousand yuan per year for the initial technology in the chemical analysis field of the aluminum-vanadium alloy production of domestic special metallurgy. The method has strong universality, improves the chemical analysis mode of the vanadium content in the aluminum-vanadium alloy in the industry, has certain reference and application values, and has wide market prospect.
Claims (10)
1. A chemical detection method for vanadium element in aluminum-vanadium alloy is characterized by comprising the following steps:
1) sampling and pretreating the aluminum-vanadium alloy: weighing a sample, placing the sample in a container, adding a hydrochloric acid solution, a nitric acid solution and water, heating for dissolving, adding a sulfuric acid solution after the sample is completely dissolved, continuously heating a phosphoric acid solution, dropwise adding nitric acid to destroy carbides, smoking until the distance between sulfur and phosphoric acid smoke is about 1-2 cm from the liquid level of the solution, taking down the mixture for cooling slightly, adding water, and cooling to room temperature;
the mass concentration of the hydrochloric acid is more than 20%; the mass concentration of the nitric acid is more than 40%; the mass concentration of the sulfuric acid is more than 70%; the mass concentration of the phosphoric acid solution is more than 70%; the upper limit is the highest concentration available on the market;
the ratio of the sample to the hydrochloric acid solution is (0.1-0.5:5-10) g/mL, the ratio of the sample to the nitric acid solution is (0.1-0.5:5-10) g/mL, the ratio of the sample to the sulfuric acid solution is (0.1-0.5:8-20) g/mL, and the ratio of the sample to the phosphoric acid solution is (0.1-0.5:5-10) g/mL;
2) calibrating an ammonium ferrous sulfate solution;
3) titration operation: dripping potassium permanganate solution into the solution obtained in the step 1) until stable red is generated, then dripping 1-2 drops of the potassium permanganate solution, uniformly mixing, standing, adding solid urea or urea solution, then dripping sodium nitrite solution to reduce excessive potassium permanganate until the solution is bright yellow, then dripping sodium nitrite solution, uniformly mixing and standing; dripping N-phenyl-o-aminobenzoic acid indicator, immediately titrating with ferrous ammonium sulfate standard solution until the color of the solution is changed from cherry red to bright green;
V3: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator;
m: weight (g) of sample.
2. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 1, characterized in that: the mass percentage concentration of the hydrochloric acid solution in the step 1) is 36-38%, the mass percentage concentration of the nitric acid solution is 65-68%, the mass percentage concentration of the sulfuric acid solution is 95-98%, and the mass percentage concentration of the phosphoric acid solution is more than 85%.
3. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 1, characterized in that: the calibration of the ammonium ferrous sulfate solution in the step 2) is as follows: absorbing potassium dichromate standard solution into a reaction container, adding sulfuric acid solution and phosphoric acid solution, adding water, cooling, dropwise adding N-phenyl anthranilic acid indicator, titrating with to-be-calibrated ammonium ferrous sulfate solution until the solution turns from rose red to bright green, and recording the volume of the consumed ammonium ferrous sulfate solution as V1; the corrected value for the N-phenylanthranilic acid indicator is V2;
the concentration of the ferrous ammonium sulfate solution is calculated according to the following formula:
c: concentration (mol/L) of potassium dichromate standard solution;
v: removing the volume (mL) of the potassium dichromate standard solution;
V1: titrating the volume (mL) of the ammonium ferrous sulfate solution consumed;
V2: corrected value (mL) for N-phenylanthranilic acid indicator.
4. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 3, characterized in that: step 2), the potassium dichromate standard solution is 0.05-0.15 mol/l; the dosage of the potassium dichromate standard solution is 8-15 mL; the volume ratio of the sulfuric acid solution to the potassium dichromate standard solution is 1: 0.8-1.2; the volume ratio of the phosphoric acid solution to the potassium dichromate standard solution is 1: 0.4-0.6.
5. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 3, characterized in that: in the step 2), the mass concentration of the sulfuric acid is more than 70%; the mass concentration of the phosphoric acid solution is more than 70%; the upper limit is the highest concentration available on the market.
6. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 3, characterized in that: in the step 2), 20mL to 100mL of water is added.
7. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 3, characterized in that: the correction of the N-phenyl-o-aminobenzoic acid indicator means that after the volume of the consumed ammonium ferrous sulfate solution obtained for the first time is V1, potassium dichromate standard solution with the same concentration and volume is added, the ammonium ferrous sulfate solution to be calibrated is continuously titrated until the solution is changed from rose red to bright green, and the difference value between the volume of the ammonium ferrous sulfate solution used for the second time and V1 is V2.
8. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 1, characterized in that: step 3), the concentration of the potassium permanganate solution is 1.0-3.5%;
the concentration of the sodium nitrite solution in the step 3) is 0.5-2%.
9. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 1, characterized in that: the concentration of the N-phenyl-o-aminobenzoic acid indicator is 0.1-0.3%.
10. The chemical detection method for vanadium element in aluminum vanadium alloy according to claim 1, characterized in that: the concentration of the ammonium ferrous sulfate standard solution in the step 3) is 0.03-0.10 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910934415.9A CN112578076A (en) | 2019-09-29 | 2019-09-29 | Chemical detection method for vanadium element in aluminum-vanadium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910934415.9A CN112578076A (en) | 2019-09-29 | 2019-09-29 | Chemical detection method for vanadium element in aluminum-vanadium alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112578076A true CN112578076A (en) | 2021-03-30 |
Family
ID=75111323
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910934415.9A Pending CN112578076A (en) | 2019-09-29 | 2019-09-29 | Chemical detection method for vanadium element in aluminum-vanadium alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112578076A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104267141A (en) * | 2014-08-29 | 2015-01-07 | 中国航空工业集团公司北京航空材料研究院 | Method for determining vanadium element in vanadium iron alloy |
| CN107436290A (en) * | 2017-09-26 | 2017-12-05 | 商洛天野高新材料有限公司 | The assay method of chromium content in a kind of vananum |
-
2019
- 2019-09-29 CN CN201910934415.9A patent/CN112578076A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104267141A (en) * | 2014-08-29 | 2015-01-07 | 中国航空工业集团公司北京航空材料研究院 | Method for determining vanadium element in vanadium iron alloy |
| CN107436290A (en) * | 2017-09-26 | 2017-12-05 | 商洛天野高新材料有限公司 | The assay method of chromium content in a kind of vananum |
Non-Patent Citations (3)
| Title |
|---|
| 上海第一钢铁厂中心试验室: "《钢铁化学分析》", 31 July 1977, 上海人民出版社 * |
| 孙宝莲 等: "高锰酸钾氧化-亚铁滴定法测定钒铝合金钒含量", 《稀有金属材料与工程》 * |
| 郑小敏 等: "钒铝合金中钒量测定方法研究", 《钢铁钒钛》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101413898B (en) | Quantitative analysis method of vanadium in high chrome alloy | |
| CN101349648B (en) | Method for measuring trace elements in high titanium high boiler slag | |
| CN102128834B (en) | Method for determining total ferrum content in chromite | |
| CN103808558B (en) | The digestion procedure of vanadium nitrogen ferrotitanium hybrid alloys core-spun yarn and detection method | |
| CN102288725A (en) | Method for measuring organic matters in soil | |
| CN101334365B (en) | Determination method for chloride ion content of temper rolling liquor for steel plate rolling | |
| CN105158406A (en) | Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method | |
| CN103344629B (en) | The ICP-AES measurement method of lead content in water | |
| Chen et al. | Tellurium speciation in a bioleaching solution by hydride generation atomic fluorescence spectrometry | |
| CN104849400B (en) | Novel method for measuring content of zinc in alkaline zinc-nickel alloy plating solution | |
| CN109596454B (en) | Method for detecting contents of moisture, vanadium pentoxide and carbon in hexamine vanadium | |
| CN102418094B (en) | Low-temperature phosphating technology for cold forming processing | |
| CN104949961A (en) | ICP-AES detecting method for content of germanium element in lead-free solder material | |
| CN105092496A (en) | Method for detecting content of phosphorus in nitrification intensifier | |
| CN112578076A (en) | Chemical detection method for vanadium element in aluminum-vanadium alloy | |
| CN110726802B (en) | Method for accurately analyzing nickel sulfate in citrate nickel plating solution | |
| CN111257503A (en) | Method for detecting chromium content of high-chromium-content aluminum alloy based on titration analysis method | |
| CN105548147A (en) | Method for determining manganese element content in rich-manganous slags | |
| CN112649557A (en) | Method for measuring zirconium content in zirconium sponge | |
| CN111380999B (en) | Analysis method for measuring high-content molybdenum element in metal material by adopting potentiometric titration | |
| CN111024679A (en) | Method for measuring chemical components in Inconel | |
| CN116990443B (en) | Accurate detection method for COD in high-chlorine low-COD water sample | |
| CN112577946A (en) | Preparation method and detection method of sample solution for determining silicon, iron, phosphorus and selenium elements in manganese and manganese alloy | |
| JP5569336B2 (en) | High purity organometallic compound analysis treatment liquid, trace impurity analysis method using the treatment liquid, and high purity organometallic compound subjected to the analysis method | |
| Shao et al. | Exploiting a simple method for the determination of manganese in polyethylene lined tubing for petroleum and natural gas industries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210330 |
|
| RJ01 | Rejection of invention patent application after publication |