CN101256150A - Method for determining vanadium in vanadium nitrogen alloy - Google Patents

Method for determining vanadium in vanadium nitrogen alloy Download PDF

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CN101256150A
CN101256150A CNA2008100156071A CN200810015607A CN101256150A CN 101256150 A CN101256150 A CN 101256150A CN A2008100156071 A CNA2008100156071 A CN A2008100156071A CN 200810015607 A CN200810015607 A CN 200810015607A CN 101256150 A CN101256150 A CN 101256150A
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董丙成
许荣昌
李西忠
王成林
闫志华
王秀花
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Laiwu Iron and Steel Co Ltd
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Laiwu Iron and Steel Co Ltd
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Abstract

The invention relates to a method for testing vanadium in vanadium-nitrogen alloy. The method has the following steps: crushing and sieving the test sample through 200 mesh, fetching the sample from the erlenmeyer flask, adding H<SUB>2</SUB>SO<SUB>4</SUB>(1+4) and dissolving it by heating, dropping nitric acid to oxidizing it, adding concentrated H<SUB>3</SUB>PO<SUB>4</SUB> and heating to the state that the sulfuric acid emits smoke, and then cooling to room temperature; adding (NH<SUB>4</SUB>)<SUB>2</SUB>Fe(SO<SUB>4</SUB>)<SUB>2</SUB> standard solution, dropping KMnO<SUB>4</SUB> solution till the test solution is red steadily and the color does not fade; adding urea solution, dropping NaNO<SUB>2</SUB> solution till the red color fades, adding NaAsO<SUB>2</SUB> solution, placing, dropping 2-3 drops of CrV indicator, immediately titrating with the ammonium ferrous sulphate standard solution till the color changes from cerise into light green, according to the volume of the consumed ammonium ferrous sulphate standard solution, calculating the content of the vanadium in the sample. The test result of the vanadium in vanadium-nitrogen alloy is accurate and the method is convenient.

Description

The assay method of vanadium in a kind of VN alloy
Technical field
The present invention relates to the quantitative test detection technique of vanadium in a kind of alloy, the quantitative test detection method of vanadium belongs to the chemical analysis detection range in particularly a kind of VN alloy.
Technical background
All do not have in all data of the present national standard of the assay method of vanadium in the relevant VN alloy to introduce, do not see record on the international standard yet.VN alloy is the comparatively ideal compound additive that a kind of alternative vanadium iron is used to produce the steel of vanadium microalloy.Vanadium nitride makes an addition to the comprehensive mechanical performances such as intensity, toughness, ductility and thermal fatigue resistance that can improve steel in the steel, and makes steel have good weldability.Reaching under the same intensity, adding vanadium nitride and save vanadium addition 30～40%, and then reduced cost.Because the content of vanadium is generally higher in the VN alloy, about about 80%, therefore, conventional analysis means difficulty is bigger greatly, the research of the arsenazo M Decoloring Spectrophotometric Determination vanadium that Chinese periodical " Guangdong University of Technology's journal " 3 phases in 2002 provide, employing be beam split range ratioing technigue.The shortcoming that existing method exists is that condition test is too complicated, and the acidity of sulfuric acid range of control is too wide, and acidity control numerical value is not concrete, and reductive agent sodium arsenite and sodium nitrite additional amount are on the low side, makes the manganic reduction not thorough, causes the result inaccurate.
Summary of the invention
The present invention mainly is the shortcoming that exists at present analytical approach, and the assay method of vanadium in a kind of VN alloy is provided.
Technical scheme of the present invention is as follows:
The assay method of vanadium in a kind of VN alloy, step is as follows:
(1) preparation of test analysis sample
After sample to be detected pulverized with disintegrating machine, be milled to granularity all by 200 mesh sieves, then sample packed in the bag, be stored in the drying basin standby through muller.
(2) reagent
Sulfuric acid: (1+4); With the sulfuric acid of 1 unit volume and the water mixed preparing of 4 unit volumes;
Nitric acid: ρ 1.42;
Phosphoric acid: ρ 1.70;
Liquor potassic permanganate: 0.5%wt; (mass percent concentration, below all with)
Iron ammonium sulfate [(NH 4) 2Fe (SO 4) 2] standard solution: 0.1000mol/L, with the preparation of (5+9) sulfuric acid; Described (5+9) sulfuric acid is with the sulfuric acid of 5 unit volumes and the water mixed preparing of 95 unit volumes.
The CrV indicator: take by weighing benzene for ortho position ammonium benzoic acid 0.2g, sodium carbonate 0.2g is dissolved in the 100ml hot water;
Urea cellulose solution: 20%wt;
Sodium nitrite solution: 2%wt;
Sodium arsenite solution: 0.0500mol/L.
(3) experimental technique
Take by weighing sample 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml, low-temperature heat dissolving, treated that bulla occurs after, drip 2～3ml nitric acid oxidation, add dense H 3PO 45ml continues to be heated to and emits sulfuric acid cigarette 2～3min, takes off, and adds entry 50ml, is cooled to room temperature.Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till.Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2～3 NaNO 2Solution, place 2min, drip 2～3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, calculate the content of vanadium in the sample by following formula:
V % = T &CenterDot; V G &times; 100
In the formula, T: the iron ammonium sulfate standard solution is to the titer of vanadium, V: the volume (ml) of the iron ammonium sulfate standard solution that is consumed, G: sample weighting amount (g).
At the method for the invention described above, specify as follows:
1. the influence of acidity
Show that by test the acidity of sulfuric acid when oxidation and titration vanadium should be controlled between the 2.5mol/L is advisable.If acidity is during less than 2mol/L, sluggish then, titration end-point is difficult to be grasped.
2. Temperature Influence
Experiment draws, and (about 25 ℃) an amount of KMnO is at room temperature carried out in the oxidation of vanadium 4Can be with V 4+Be oxidized to V quantitatively 5+, and this moment is to Cr 3+Oxidation rate but extremely slow.If the temperature of test solution is too high, in vanadium oxide, Cr 3+Also oxidized, cause analysis vanadium result higher.
3. the addition of iron ammonium sulfate:
At room temperature add a certain amount of iron ammonium sulfate and can eliminate the interference of high valence chrome and oxygenant thereof, generally speaking, can be per sample in chromium content and decide.Show by experiment, during vanadium, add iron ammonium sulfate standard solution 2ml in measuring VN alloy, can eliminate it and disturb, at this moment the color of test solution should be blue-green.
4. the consumption of potassium permanganate:
At ambient temperature, KMnO 4Though the speed of chromium oxide is very slow, because oxidation rate and the content of chromium, the consumption of potassium permanganate, the acidity of test solution add KMnO in addition 4After standing time and test solution temperature very big relation is arranged, therefore dripping KMnO 4During vanadium oxide, do not want excessive too much, otherwise a large amount of potassium permanganate also can make analysis result higher the chromium oxidation.General require to drip to be to test solution stablize redness and do not take off and be advisable.
5. the consumption of sodium nitrite:
Before dripping sodium nitrite, should add a certain amount of urea cellulose solution earlier, because an amount of sodium nitrite can reduce manganese at high price, do not reduce vanadium at high price.Excessive sodium nitrite is used the plain destruction of urea.Therefore in dropping to test solution after red the disappearance, and excessive 4-5 drips, and shows that manganese has been reduced fully, and eliminated the interference of high price manganese.
6. the consumption of sodium arsenite
Add a spot of sodium arsenite and can optionally reduce high valence chrome, but in sodium arsenite reduction high valence chrome, induce subsidiary reaction, promptly the part bivalent manganese is oxidized to trivalent by high valence chrome, therefore when adding the 5ml sodium arsenite, need add 2 sodium nitrites with the reduction manganic.Its reaction is as follows:
Figure A20081001560700042
Mn 2(SO 4) 3+NaNO 2+H 2O＝2MnSO 4+NaNO 3+H 2SO 4
7.CrV the influence of indicator:
Itself has oxidation-reduction quality indicator solution.Test factually, every indicator solution is equivalent to the iron ammonium sulfate mark liquid 0.12ml of 0.0025mol/L, and therefore addition should be consistent in operation, is advisable for general 2～3.To reduce the error that this respect is former thereby cause.
8. when titration closes on terminal point, should shake, titration simultaneously should be slow, otherwise excessive easily more.
Technical characterstic of the present invention is to adopt the method for deciding, test from the conditions such as addition of the consumption of the decomposition of sample, reagent and various reductive agent, oxygenant, be easy to redox characteristics at room temperature based on vanadium, test solution under room temperature with potassium permanganate optionally vanadium oxide and the principle of chromium oxide not, with ferrous titration vanadium amount, obtained satisfied result.The assay method of vanadium is simple to operate, quick in the VN alloy of the present invention, accurately, adapts to the needs of producing, and can in time provide to Iron and Steel Production and analyze data accurately.
The invention solves the technical matters of the assay method of vanadium in the VN alloy, filled up the blank in the assay method field of vanadium in the VN alloy.VN alloy belongs to scarce resource; cost an arm and a leg; the accurate vanadium of measuring in the VN alloy helps iron and steel enterprise and economizes on resources; the protection environment; China is Iron and Steel Production big country, and the performance reduction iron and steel output that improves steel is an inexorable trend, and micro-alloy high-strength steel widely applies the VN alloy of stable performance as the reinforcement means; therefore, the present invention has broad application prospects.
Embodiment
The present invention will be further described below in conjunction with embodiment, but be not limited thereto.
Specimen is after VN alloy sample to be determined is pulverized with disintegrating machine, to be milled to granularity all by 200 mesh sieves through muller in following examples.Used medicine and reagent are as follows:
Sulfuric acid (1+4) is with the sulfuric acid of 1 unit volume and the water mixed preparing of 4 unit volumes;
Nitric acid ρ 1.42;
Phosphoric acid ρ 1.70;
Liquor potassic permanganate: 0.5%wt;
Iron ammonium sulfate [(NH 4) 2Fe (SO 4) 2] standard solution: 0.1000mol/L, with the preparation of (5+9) sulfuric acid; Described (5+9) sulfuric acid is with the sulfuric acid of 5 unit volumes and the water mixed preparing of 95 unit volumes.
The CrV indicator: take by weighing benzene for ortho position ammonium benzoic acid 0.2g, sodium carbonate 0.2g is dissolved in the 100ml hot water;
Urea cellulose solution: 20%wt;
Sodium nitrite solution: 2%wt;
Sodium arsenite solution: 0.0500mol/L.
Embodiment 1:
Take by weighing vanadium iron standard model (being numbered 69-44) 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml places on the electric furnace low-temperature heat dissolving, treated that bulla occurs after, drip the 2-3ml nitric acid oxidation, add H 3PO 4(dense) 5ml continues to be heated on the electric furnace and emits sulfuric acid cigarette 2-3min, takes off coldly slightly, adds entry 50ml, is cooled to room temperature.Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till.Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2 NaNO 2Solution is placed 2min, drips 3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, carry out calculating as a result by following formula, obtain the content of vanadium in the sample:
V % = T &CenterDot; V G &times; 100
In the formula, T: the iron ammonium sulfate standard solution is to the titer of vanadium, V: the volume (ml) of the iron ammonium sulfate standard solution that is consumed, G: sample weighting amount (g).
The results are shown in Table 1.
Embodiment 2:
Take by weighing vanadium iron standard model (being numbered 50-A-2) 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml places on the electric furnace low-temperature heat dissolving, treated that bulla occurs after, drip the 2-3ml nitric acid oxidation, add H 3PO 4(dense) 5ml continues to be heated on the electric furnace and emits sulfuric acid cigarette 2-3min, takes off coldly slightly, adds entry 50ml, is cooled to room temperature.Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till.Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2 NaNO 2Solution, place 2min, drip 3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, calculate the content of vanadium in the sample with the method for embodiment 1.The results are shown in Table 1.
Embodiment 3:
Take by weighing VN alloy sample (being numbered 1#) 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml places on the electric furnace low-temperature heat dissolving, treated that bulla occurs after, drip the 2-3ml nitric acid oxidation, add H 3PO 4(dense) 5ml continues to be heated on the electric furnace and emits sulfuric acid cigarette 2-3min, takes off coldly slightly, adds entry 50ml, is cooled to room temperature.Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till.Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2 NaNO 2Solution, place 2min, drip 3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, calculate the content of vanadium in the sample with the method for embodiment 1.The results are shown in Table 1.
Embodiment 4:
Take by weighing VN alloy sample (being numbered 2#) 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml places on the electric furnace low-temperature heat dissolving, treated that bulla occurs after, drip the 2-3ml nitric acid oxidation, add H 3PO 4(dense) 5ml continues to be heated on the electric furnace and emits sulfuric acid cigarette 2-3min, takes off coldly slightly, adds entry 50ml, is cooled to room temperature.Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till.Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2 NaNO 2Solution, place 2min, drip 3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, calculate the content of vanadium in the sample with the method for embodiment 1.The results are shown in Table 1.
Table 1. test result
The standard model numbering Standard value % This law measured value % Error
69-44 44.04 44.01 -0.03
50-A-2 52.82 52.81 -0.01
The 1# VN alloy 79.55 79.59 0.04
The 2# VN alloy 80.34 80.27 -0.07

Claims (1)

1. the assay method of vanadium in the VN alloy, step is as follows:
(1) testing sample is pulverized with disintegrating machine after, be milled to granularity all by 200 mesh sieves through muller, then sample is packed in the bag, be stored in the drying basin standby;
(2) medicine and reagent
Sulfuric acid (1+4) is with the sulfuric acid of 1 unit volume and the water mixed preparing of 4 unit volumes;
Nitric acid ρ 1.42;
Phosphoric acid ρ 1.70;
Liquor potassic permanganate 0.5%wt;
Iron ammonium sulfate [(NH 4) 2Fe (SO 4) 2] standard solution: 0.1000mol/L, with the preparation of ((with the sulfuric acid of 5 unit volumes and the water mixed preparing of 95 unit volumes)) sulfuric acid;
The CrV indicator: take by weighing benzene for ortho position ammonium benzoic acid 0.2g, sodium carbonate 0.2g is dissolved in the 100ml hot water;
Urea cellulose solution 20%wt;
Sodium nitrite solution 2%wt;
Sodium arsenite solution 0.0500mol/L;
(3) take by weighing sample 0.2000g in the Erlenmeyer flask of 500ml, add H 2SO 4(1+4) 50ml, low-temperature heat dissolving, treated that bulla occurs after, drip 2～3ml nitric acid oxidation, add dense H 3PO 45ml continues to be heated to and emits sulfuric acid cigarette 2～3min, takes off, and adds entry 50ml, is cooled to room temperature; Add (NH 4) 2Fe (SO 4) 2Standard solution 2ml after shaking up, places 2min, drips KMnO 4Solution to test solution be stablize redness and do not take off till; Place 2min, add urea cellulose solution 10ml, drip NaNO 2Solution disappears to red, and excessive 2, add NaAsO 2Behind the solution 5ml, add 2～3 NaNO 2Solution, place 2min, drip 2～3 of CrV indicator, becoming bright green to test solution by cherry-red with the iron ammonium sulfate standard solution titration immediately is terminal point, according to the volume of the iron ammonium sulfate standard solution that is consumed, calculate the content of vanadium in the sample by following formula:
V % = T &CenterDot; V G &times; 100
In the formula, T: the iron ammonium sulfate standard solution is to the titer of vanadium, V: the volume (ml) of the iron ammonium sulfate standard solution that is consumed, G: sample weighting amount (g).
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101424644B (en) * 2008-12-12 2011-05-04 江西稀有稀土金属钨业集团有限公司 Vanadium content measuring method in vanadium-added or chromium-vanadium-added tungsten basal body
CN102507556A (en) * 2011-10-31 2012-06-20 攀钢集团江油长城特殊钢有限公司 Method for measuring vanadium content of silicon ferrovanadium
CN102928425A (en) * 2012-10-31 2013-02-13 攀枝花钢城集团瑞钢工业有限公司 Method for determining vanadium in silicon-vanadium alloy
CN103091450A (en) * 2013-01-02 2013-05-08 河北钢铁股份有限公司承德分公司 Method for rapidly determining content of total iron in nitrided ferrovanadium
CN103134797A (en) * 2013-01-28 2013-06-05 河北钢铁股份有限公司承德分公司 Measuring method of tetravalent vanadium contents in vanadium oxide
CN103344472A (en) * 2013-07-11 2013-10-09 山东省冶金科学研究院 Vanadium-nitrogen alloy standard sample for chemical analysis and preparation method thereof
CN103837532A (en) * 2012-11-21 2014-06-04 山东兴盛矿业有限责任公司 Method for rapidly accurately measuring vanadium in vanadium-titanium iron powder
CN104181158A (en) * 2014-08-22 2014-12-03 武钢集团昆明钢铁股份有限公司 Method for measuring concentration of tetravalent and pentavalent vanadium ions in vanadium battery electrolyte
CN110849872A (en) * 2019-12-04 2020-02-28 河钢股份有限公司承德分公司 Method for determining vanadium in high-content ferrovanadium alloy
CN113984866A (en) * 2021-11-11 2022-01-28 承德建龙特殊钢有限公司 Method for measuring vanadium content in vanadium-nitrogen alloy

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101424644B (en) * 2008-12-12 2011-05-04 江西稀有稀土金属钨业集团有限公司 Vanadium content measuring method in vanadium-added or chromium-vanadium-added tungsten basal body
CN102507556A (en) * 2011-10-31 2012-06-20 攀钢集团江油长城特殊钢有限公司 Method for measuring vanadium content of silicon ferrovanadium
CN102928425A (en) * 2012-10-31 2013-02-13 攀枝花钢城集团瑞钢工业有限公司 Method for determining vanadium in silicon-vanadium alloy
CN103837532A (en) * 2012-11-21 2014-06-04 山东兴盛矿业有限责任公司 Method for rapidly accurately measuring vanadium in vanadium-titanium iron powder
CN103091450A (en) * 2013-01-02 2013-05-08 河北钢铁股份有限公司承德分公司 Method for rapidly determining content of total iron in nitrided ferrovanadium
CN103134797A (en) * 2013-01-28 2013-06-05 河北钢铁股份有限公司承德分公司 Measuring method of tetravalent vanadium contents in vanadium oxide
CN103344472A (en) * 2013-07-11 2013-10-09 山东省冶金科学研究院 Vanadium-nitrogen alloy standard sample for chemical analysis and preparation method thereof
CN103344472B (en) * 2013-07-11 2016-04-27 山东省冶金科学研究院 A kind of chemical analysis VN alloy standard model and preparation method thereof
CN104181158A (en) * 2014-08-22 2014-12-03 武钢集团昆明钢铁股份有限公司 Method for measuring concentration of tetravalent and pentavalent vanadium ions in vanadium battery electrolyte
CN110849872A (en) * 2019-12-04 2020-02-28 河钢股份有限公司承德分公司 Method for determining vanadium in high-content ferrovanadium alloy
CN113984866A (en) * 2021-11-11 2022-01-28 承德建龙特殊钢有限公司 Method for measuring vanadium content in vanadium-nitrogen alloy

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