CN103091450A - Method for rapidly determining content of total iron in nitrided ferrovanadium - Google Patents
Method for rapidly determining content of total iron in nitrided ferrovanadium Download PDFInfo
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- CN103091450A CN103091450A CN2013100002303A CN201310000230A CN103091450A CN 103091450 A CN103091450 A CN 103091450A CN 2013100002303 A CN2013100002303 A CN 2013100002303A CN 201310000230 A CN201310000230 A CN 201310000230A CN 103091450 A CN103091450 A CN 103091450A
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Abstract
The invention discloses a method for rapidly determining the content of total iron in nitrided ferrovanadium. The method comprises the steps of: 1, decomposing a nitrided ferrovanadium sample by an alkali fusion method to obtain an alkali fusion sample; 2, leaching the alkali fusion sample by hydrochloric acid, adding sodium hydroxide to a leaching solution for precipitation, and filtering and separating the solution to obtain a ferric hydroxide precipitate; 3, acidifying the ferric hydroxide participate by hydrochloric acid, heating the acidified precipitate to a boiling point, dropwise adding stannous chloride to the heated precipitate to reduce ferric iron into ferrous until the stannous chloride is excessive; and 4, oxidizing the excessive stannous chloride by mercuric chloride, titrating the oxidized stannous chloride by a potassium dichromate standard solution with sodium diphenylaminesulfonate being an indicator, thus calculating the content of the total iron of the nitrided ferrovanadium sample. The method is capable of separating vanadium and ferrum and eliminating interference of high vanadium to determination of the total iron, thereby ensuring the accuracy of a determination result. The method is used for directly determining the content of the total iron in the nitrided ferrovanadium, the detection time is shortened from original 10h to 1h, and the detection speed is greatly enhanced. The method has the characteristics of being direct, simple, convenient and feasible.
Description
Technical field
The present invention relates to a kind of method of measuring iron content in alloy, the method for all iron content in especially a kind of Fast Measurement ferrovanadium nitride.
Background technology
Along with the exploitation of vanadium-containing steel, receive much concern as the full composition of ferrovanadium nitride of steel smelt additive.In recent years, in the check work of the full composition of ferrovanadium nitride, the component content of vanadium detects the method for existing comparative maturity, the assay method of the assay method of a kind of vanadium in vanadium nitrogen alloy of providing of number of patent application 200810015607.1, a kind of vanadium in vanadium nitrogen alloy that number of patent application 201110193060.6 provides for example, and the detection method of full iron (TFe) content rarely has report.Find through looking into interrelated data, see for the research of full iron assay method in VN alloy " mensuration of full iron in vanadium titano-magnetite and rich vanadium product---the molten sample of phosphoric acid does not separate vanadium and surveys iron " that thoughtful being distal to of only having Panzhihua Iron and Steel Group company " Sichuan is metallurgical " 01 phase of nineteen eighty-two of report delivers, this full iron assay method adopts the molten sample of phosphoric acid not separate vanadium and surveys iron.Though ferrovanadium nitride belongs to VN alloy, because content of vanadium in ferrovanadium nitride is very high, and there is similarity in vanadium, iron chemical property, thus do not separate high vanadium measure all iron content operating conditions and as a result accuracy all be difficult to hold.And at present for the multiplex indirect minusing of the detection of all iron content in ferrovanadium nitride, namely first measure the wherein content of major component vanadium, the methods such as manual chemistry or ICP spectrometer that recycle are measured the content of other impurity elements, and the content that then deducts vanadium, nitrogen content and other impurity elements with total content namely gets all iron content.This method need to be measured a plurality of elements, complex operation, and time-consuming taking a lot of work is difficult to obtain accurate result, more can not provide qualitative data for production in time.
In sum, at present for the detection of all iron content in ferrovanadium nitride, under the prerequisite that guarantees the measurement result accuracy, there is no directly fast method can follow.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for all iron content in the high Fast Measurement ferrovanadium nitride of a kind of favorable reproducibility, accuracy.
For solving the problems of the technologies described above, determination step that the present invention takes is: (1) adopts alkali fusion to decompose the ferrovanadium nitride sample, obtains the alkali fusion sample;
(2) adopt hydrochloric acid leaching alkali fusion sample, add NaOH to precipitate in leaching liquid, isolated by filtration obtains ferric hydroxide precipitate;
(3) with ferric hydroxide precipitate with hcl acidifying after, be heated to boiling point, drip stannous chloride ferric iron be reduced to ferrous iron to excessive;
(4) adopt the excessive stannous chloride of mercuric chloride oxidation, fixed with potassium dichromate mark drop then take diphenylamine sulfonic acid sodium salt as indicator, utilize formula (A) to calculate the full iron amount W of ferrovanadium nitride sample
TFe
（A）
In formula:
The concentration of c-potassium dichromate standard solution, mol/L;
The volume of the potassium dichromate standard solution that consumes during V-titration sample, mL;
V
0-titration consumes the volume of potassium dichromate standard solution, mL in company with sample blank;
The quality of m-sample, g;
M
FeThe molal weight of-iron, g/mol.
Alkali fusion in step of the present invention (1) adopts the first low temperature fritting method of high-temperature fusion again.Described alkali fusion is: in the high alumina crucible, the ferrovanadium nitride sample is mixed with flux, then in 200～300 ℃ of fritting, after solid all melts in crucible, in 700～800 ℃ of melting 10～15min.Described melt temperature is 700 ℃.Described flux is sodium carbonate, NaOH and/or sodium peroxide; Ferrovanadium nitride sample and flux mass ratio are 1:40～1:20; First with flux and the ferrovanadium nitride sample mixing of 60%～70% weight, then will remain flux and cover thereon.
Hydrochloric acid in step of the present invention (2) is for analyzing pure concentrated hydrochloric acid, and every gram ferrovanadium nitride adds hydrochloric acid 100～150mL.Described NaOH is the sodium hydroxide solution of mass percent concentration 20%～80%, and every gram ferrovanadium nitride adds NaOH 100～150mL.The concentration of described sodium hydroxide solution is preferably 50%.
Hydrochloric acid in step of the present invention (3) is for analyzing pure concentrated hydrochloric acid, and every gram ferrovanadium nitride adds hydrochloric acid 100～150mL.Ferric iron is reduced to ferrous iron entirely when stannous chloride drops to solution by faint yellow becoming colorless, and described stannous chloride is excessive 1～2mL preferably.
The beneficial effect that adopts technique scheme to produce is: (1) the present invention first utilizes alkali fusion to melt sample, recycling hydrochloric acid and NaOH, and namely separable vanadium, iron, get rid of the interference that high vanadium is measured full iron, thereby guarantee the measurement result accuracy; Compare with the minusing of complex operation, the inventive method becomes direct mensuration with the detection of all iron content in ferrovanadium nitride by indirect determination, shortened to 1 hour by original 10 hours detection time, increase substantially detection speed, and provide a kind of directly easy, practicable method for the detection of all iron content in ferrovanadium nitride.
(2) at the catabolic phase of sample, compare with the direct melting of traditional high temperature, the present invention adopts the first low temperature fritting sample-smelting method of high-temperature fusion again, controls reaction velocity, has prevented that effectively the molten sample of ferrovanadium nitride from splashing, and avoids molten sample loss.
(3) getting rid of the interference stage of high vanadium to full iron mensuration, the present invention replaces the secondary filtration method of water logging crucible with a filtration method of acidleach crucible, in the situation that can get rid of equally high vanadium, iron is disturbed, and has simplified operation steps, has saved manpower and material consumption.
(4) at ferric reduction phase, the present invention controls heating condition for only being heated to boiling point, has prevented that effectively lower boiling ferric trichloride from volatilizing and finally having avoided measurement result on the low side.
Embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment.
Embodiment 1: in this Fast Measurement ferrovanadium nitride, the processing step of the method for all iron content is as described below.
(1) decomposition of sample: take the 0.2000g Sample A in the high alumina crucible that fills in advance the 3g sodium peroxide, high alumina crucible volume is 30mL, mixing, cover again upper 2g sodium peroxide, it is positioned over heating and melting on 250 ℃ of electric furnaces, after solid all melts in crucible, is transferred to melting 10min in 700 ℃ of muffle furnaces, take out slightly coldly, obtain the alkali fusion sample;
(2) get rid of the interference that high vanadium is measured full iron: the crucible after will be above-mentioned slightly cold is put into the 400mL beaker of containing in advance the 20mL pure concentrated hydrochloric acid of analysis (massfraction 36～38%) and is leached sample, washes out crucible, obtains leaching liquid; The NaOH that adds 20mL, 50wt% in the leaching liquid, until precipitation fully after, filter with the middling speed quantitative filter paper, wash beaker with water 3 times, washing precipitation 6 times obtains ferric hydroxide precipitate;
(3) ferric reduction: analyze pure concentrated hydrochloric acid (massfraction 36～38%) with 20mL ferric hydroxide precipitate is washed in beaker, solution is heated to little boiling, under agitation, drip stannous chloride solution and disappear to yellow, and excessive 1mL; Wherein the mass percentage concentration of stannous chloride solution is 10%, is formulated as follows: take the 10g stannous chloride and be dissolved in the hot hydrochloric acid of 20mL, be diluted with water to 100mL, mixing;
(4) mensuration of full iron: flowing water is cooled to room temperature, add the saturated liquor hydrargyri perchloridi of 10mL, mixing, standing 2 min, be diluted with water to approximately 150mL, add 20mL mixture of sulfuric phosphoric acid (3+3+14), two diphenylamine sulfonic acid sodium solutions, using immediately potassium dichromate standard solution (0.01mol/L) to be titrated to stable purple and placing 15s colour-fast is terminal point, and record consumes the volume V of potassium dichromate standard solution; Wherein the mass percentage concentration of diphenylamine sulfonic acid sodium solution is 1%, is formulated as follows: take the 1g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL sulfuric acid (1+99);
(5) blank analysis: analyze simultaneously with sample, but without the decomposition step of sample, get rid of the interference that high vanadium measures full iron identical with sample analysis with ferric reduction step.In the mensuration stage of full iron, after flowing water is cooled to room temperature, add 10.00 mL iron ammonium sulfate standards molten (0.01mol/L) in solution, and then add the saturated liquor hydrargyri perchloridi of 10mL, mixing, standing 1～3min, preferred 2min, be diluted with water to approximately 150mL, add 15～30mL mixture of sulfuric phosphoric acid (3+3+14), preferred 20mL, the diphenylamine sulfonic acid sodium solution of two 1%, using immediately potassium dichromate standard solution (0.01mol/L) to be titrated to stable purple and placing 15s colour-fast is terminal point, writes down the volume V that consumes the potassium dichromate standard solution
1Add 10.00 mL iron ammonium sulfate standard solution (0.01mol/L) again in solution, using immediately potassium dichromate standard solution (0.01mol/L) to be titrated to stable purple and placing 15s colour-fast is terminal point, writes down the volume V that consumes the potassium dichromate standard solution
2, blank value V
0=V
1-V
2
(6) calculating of all iron content: utilize the percentage composition of the full iron of formula calculating,
In formula:
The concentration of c-potassium dichromate standard solution, mol/L;
The volume of the potassium dichromate standard solution that consumes during V-titration sample, mL;
V
0-titration consumes the volume of potassium dichromate standard solution, mL in company with sample blank;
The quality of m-sample, g;
55.85-the molal weight of iron, g/mol.
After measured, in this example, the amount of ferrovanadium nitride sample consumption potassium dichromate standard solution is 14.20mL, and the blank amount that consumes the potassium dichromate standard solution is 0.10mL, and the content that can be calculated full iron in this routine ferrovanadium nitride according to formula (A) is 23.62%.
Embodiment 2: in this Fast Measurement ferrovanadium nitride, the processing step of the method for all iron content is as described below.
(1) decomposition of sample: take the 0.1500g sample B in the high alumina crucible that fills in advance 2g sodium carbonate and NaOH (mass ratio 1:1) mixed flux, mixing, cover again the upper above-mentioned mixed flux of 1g, it is positioned over heating and melting on 300 ℃ of electric furnaces, after solid all melts in crucible, be transferred to melting 15min in 750 ℃ of muffle furnaces, take out slightly cold;
(2) get rid of the interference that high vanadium is measured full iron: the crucible after will be above-mentioned slightly cold is put into the 400mL beaker of containing in advance the pure concentrated hydrochloric acid of 22.5mL analysis and is leached sample, wash out crucible, the NaOH that adds 18mL, 80wt% in the gained solution, after precipitation is complete, filter with the middling speed quantitative filter paper, wash beaker with water 3 times, washing precipitation 5 times;
(3) ferric reduction: analyze pure concentrated hydrochloric acid with 18mL ferric hydroxide precipitate is washed in beaker, solution is heated to little boiling, under agitation, drip stannous chloride solution and disappear to yellow, and excessive 2mL;
(4) mensuration of full iron: flowing water is cooled to room temperature, add the saturated liquor hydrargyri perchloridi of 10mL, mixing, standing 3min, be diluted with water to approximately 150mL, add 25mL mixture of sulfuric phosphoric acid (3+3+14), two diphenylamine sulfonic acid sodium solutions, using immediately potassium dichromate standard solution (0.01mol/L) to be titrated to stable purple and placing 15s colour-fast is terminal point, and record consumes the volume V of potassium dichromate standard solution;
Blank analysis is identical with embodiment 1 with computation process.
After measured, in this example, the amount of ferrovanadium nitride sample consumption potassium dichromate standard solution is 10.90mL, and the blank amount that consumes the potassium dichromate standard solution is 0.10mL, and the content that can be calculated full iron in this routine ferrovanadium nitride according to formula (A) is 24.13%.
Embodiment 3: in this Fast Measurement ferrovanadium nitride, the processing step of the method for all iron content is as described below.
(1) decomposition of sample: take 0.2500g sample C in the high alumina crucible that fills in advance 7g sodium carbonate and sodium peroxide (mass ratio 1:1) mixed flux, mixing, cover again upper 3g mixed flux, it is positioned over heating and melting on 200 ℃ of electric furnaces, after solid all melts in crucible, be transferred to melting 12min in 800 ℃ of muffle furnaces, take out slightly cold;
(2) get rid of the interference that high vanadium is measured full iron: the crucible after will be above-mentioned slightly cold is put into the 400mL beaker of containing in advance the pure concentrated hydrochloric acid of 30mL analysis and is leached sample, wash out crucible, add 37.5mL, 20% NaOH in the gained solution, after precipitation is complete, filter with the middling speed quantitative filter paper, wash beaker with water 3 times, washing precipitation 6 times;
(3) ferric reduction: analyze pure concentrated hydrochloric acid with 37.5mL ferric hydroxide precipitate is washed in beaker, solution is heated to little boiling, under agitation, drip stannous chloride solution and disappear to yellow, and excessive 1.5mL;
(4) mensuration of full iron: flowing water is cooled to room temperature, add the saturated liquor hydrargyri perchloridi of 10mL, mixing, standing 3min, be diluted with water to approximately 150mL, add 30mL mixture of sulfuric phosphoric acid (3+3+14), two diphenylamine sulfonic acid sodium solutions, using immediately potassium dichromate standard solution (0.01mol/L) to be titrated to stable purple and placing 15s colour-fast is terminal point, and record consumes the volume V of potassium dichromate standard solution;
Blank analysis is identical with embodiment 1 with computation process.
After measured, in this example, the amount of ferrovanadium nitride sample consumption potassium dichromate standard solution is 16.75mL, and the blank amount that consumes the potassium dichromate standard solution is 0.10mL, and the content that can be calculated full iron in this routine ferrovanadium nitride according to formula (A) is 22.32%.
Accuracy and precision test: according to embodiment 1 method, choose 1 vanadium iron standard specimen (ECRM591-1) and 4 ferrovanadium nitride samples, measure respectively 8 times, carry out accuracy and the precision test of method, analysis result sees Table 1.
Table 1: method accuracy and precision test analysis result
As can be seen from the above table, this method only-0.10% is measured vanadium iron standard specimen determination data 14.49% and standard value 14.59% deviation, and the relative standard deviation of each sample all very low (＜0.4%), illustrates that this method has higher veracity and precision.
Claims (10)
1. the method for all iron content in a Fast Measurement ferrovanadium nitride, is characterized in that, the determination step of the method is: (1) adopts alkali fusion to decompose the ferrovanadium nitride sample, obtains the alkali fusion sample;
(2) adopt hydrochloric acid leaching alkali fusion sample, add NaOH to precipitate in leaching liquid, isolated by filtration obtains ferric hydroxide precipitate;
(3) with ferric hydroxide precipitate with hcl acidifying after, be heated to boiling point, drip stannous chloride ferric iron be reduced to ferrous iron to excessive;
(4) adopt the excessive stannous chloride of mercuric chloride oxidation, fixed with potassium dichromate mark drop then take diphenylamine sulfonic acid sodium salt as indicator, utilize formula (A) to calculate the full iron amount W of ferrovanadium nitride sample
TFe
（A）
In formula:
The concentration of c-potassium dichromate standard solution, mol/L;
The volume of the potassium dichromate standard solution that consumes during V-titration sample, mL;
V
0-titration consumes the volume of potassium dichromate standard solution, mL in company with sample blank;
The quality of m-sample, g;
M
FeThe molal weight of-iron, g/mol.
2. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 1 is characterized in that: the alkali fusion in described step (1) adopts the first low temperature fritting method of high-temperature fusion again.
3. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 2, it is characterized in that, described alkali fusion is: in the high alumina crucible, the ferrovanadium nitride sample is mixed with flux, then in 200～300 ℃ of fritting, after solid all melts in crucible, in 700～800 ℃ of melting 10～15min.
4. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 3, it is characterized in that: described melt temperature is 700 ℃.
5. the method for all iron content according to claim 3 or 4 described Fast Measurement ferrovanadium nitrides, it is characterized in that: described flux is sodium carbonate, NaOH and/or sodium peroxide; Ferrovanadium nitride sample and flux mass ratio are 1:40～1:20; First with flux and the ferrovanadium nitride sample mixing of 60%～70% weight, then will remain flux and cover thereon.
6. the method for all iron content according to claim 1-4 described Fast Measurement ferrovanadium nitrides of any one is characterized in that: the hydrochloric acid in described step (2) is for analyzing pure concentrated hydrochloric acid, and every gram ferrovanadium nitride adds hydrochloric acid 100～150mL.
7. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 6, it is characterized in that: the NaOH in described step (2) is the sodium hydroxide solution of mass percent concentration 20%～80%, and every gram ferrovanadium nitride adds NaOH 100～150mL.
8. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 7, it is characterized in that: the concentration of described sodium hydroxide solution is 50%.
9. the method for all iron content according to claim 1-4 described Fast Measurement ferrovanadium nitrides of any one is characterized in that: the hydrochloric acid in described step (3) is for analyzing pure concentrated hydrochloric acid, and every gram ferrovanadium nitride adds hydrochloric acid 100～150mL.
10. the method for all iron content in Fast Measurement ferrovanadium nitride according to claim 9 is characterized in that: in described step (3), and the excessive 1～2mL of stannous chloride.
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Cited By (7)
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| CN104007227A (en) * | 2014-06-24 | 2014-08-27 | 武钢集团昆明钢铁股份有限公司 | Method for testing total iron content in vanadium slag |
| CN104391077A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining total iron in vanadium titano-magnetite by using acid dissolution method |
| CN108152101A (en) * | 2017-12-20 | 2018-06-12 | 新疆昆玉钢铁有限公司 | One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride |
| CN110794084A (en) * | 2019-11-19 | 2020-02-14 | 攀枝花钢企欣宇化工有限公司 | Method for measuring calcium chlorate content |
| CN110823868A (en) * | 2019-10-21 | 2020-02-21 | 南京钢铁股份有限公司 | Analysis method for determining primary and secondary components in composite vanadium-nitrogen alloy |
| CN111504751A (en) * | 2020-06-03 | 2020-08-07 | 中华人民共和国京唐港海关 | Sample pretreatment method for determining total iron content |
| CN114354838A (en) * | 2021-12-15 | 2022-04-15 | 中国科学院大连化学物理研究所 | Method for measuring concentration of iron and vanadium ions in mixed solution |
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| CN104007227A (en) * | 2014-06-24 | 2014-08-27 | 武钢集团昆明钢铁股份有限公司 | Method for testing total iron content in vanadium slag |
| CN104007227B (en) * | 2014-06-24 | 2016-06-01 | 武钢集团昆明钢铁股份有限公司 | The measuring method of all iron content in a kind of vanadium slag |
| CN104391077A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining total iron in vanadium titano-magnetite by using acid dissolution method |
| CN108152101A (en) * | 2017-12-20 | 2018-06-12 | 新疆昆玉钢铁有限公司 | One thermal conductivity method of inert gas fusion measures nitrogen content sample-smelting method in ferrovanadium nitride |
| CN110823868A (en) * | 2019-10-21 | 2020-02-21 | 南京钢铁股份有限公司 | Analysis method for determining primary and secondary components in composite vanadium-nitrogen alloy |
| CN110794084A (en) * | 2019-11-19 | 2020-02-14 | 攀枝花钢企欣宇化工有限公司 | Method for measuring calcium chlorate content |
| CN111504751A (en) * | 2020-06-03 | 2020-08-07 | 中华人民共和国京唐港海关 | Sample pretreatment method for determining total iron content |
| CN114354838A (en) * | 2021-12-15 | 2022-04-15 | 中国科学院大连化学物理研究所 | Method for measuring concentration of iron and vanadium ions in mixed solution |
| CN114354838B (en) * | 2021-12-15 | 2023-08-08 | 中国科学院大连化学物理研究所 | Method for measuring concentration of iron and vanadium ions in mixed solution |
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Application publication date: 20130508 |