CN109682926A - The method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy - Google Patents
The method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy Download PDFInfo
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Abstract
The invention belongs to analytical chemistry fields, and in particular to the method for continuously measuring of vanadium chromium content in a kind of vanadium chromium hydrogen bearing alloy.It can not be suitable for measuring the vanadium chromium vanadium chromium hydrogen bearing alloy for existing vanadium chromium content method for continuously measuring, the problem of measurement result inaccuracy, the present invention provides a kind of method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy, comprising the following steps: a, using sulfuric acid, nitric acid and acid decomposed by phosphoric acid sample；B, prepare liquid is restored；C, prepare liquid is aoxidized；D, content of vanadium interference is eliminated；E, content of vanadium is measured；F, vanadium oxide chromium；G, vanadium chromium content is measured.Initiative of the invention devises a kind of method for continuously measuring for vanadium high chrome contents high in alloy, has widened the scope of application of vanadium, chromium mark feed method, can be suitable for the high vanadium chromium hydrogen bearing alloy of vanadium, chromium content, and measurement result is accurate and reliable, is suitable for promoting.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to the METHOD FOR CONTINUOUS DETERMINATION side of vanadium chromium content in a kind of vanadium chromium hydrogen bearing alloy
Method.
Background technique
Currently, vanadium chromium method for continuously measuring is mainly for the vanadium and chromium progress METHOD FOR CONTINUOUS DETERMINATION in steel and alloy, sample vanadium
Content is less high, and content of vanadium is less than 6%, and chromium content is less than 12%.Use is substantially all in the operation of METHOD FOR CONTINUOUS DETERMINATION vanadium and chromium
This poisonous drugs of sodium arsenite has been arrived, has had great harm to human body and environment；It is generally first by method in the prior art
Survey the resultant that content of vanadium measures vanadium and chromium again.Regardless of method, if vanadium and when all high chromium content in sample, measurement
It can all be influenced by chromium content when content of vanadium, positive interference can be generated, it is necessary to which the interference for eliminating chromium just can ensure that the standard of vanadium measurement
True property, so that it is guaranteed that the accuracy of chrome determination.Vanadium and chromium content are high in vanadium chromium hydrogen bearing alloy, content of vanadium 40~65%,
Chromium content 10~25%, is found by experiment that, surveying vanadium chromium resultant again using existing first measurement vanadium, (vanadium and chromium of high price can be with
Redox reaction occurs for ferrous iron, and same titration standard liquid can only could be changed colour after vanadium and chromium are all reduced with an indicator and be referred to
Show terminal, so can only measure to obtain vanadium chromium content, subtract content of vanadium, can just obtain chromium content) method be not able to satisfy vanadium chromium
The METHOD FOR CONTINUOUS DETERMINATION of vanadium chromium content in hydrogen bearing alloy, is mainly manifested in: vanadium measurement content is higher, silver nitrate, persulfuric acid when measuring chromium
When ammonium dosage is improper, it is difficult for vanadium chromium to be fully oxidized to high price, causes vanadium chromium resultant Lower result.
Summary of the invention
The technical problem to be solved in the present invention are as follows: existing vanadium chromium content method for continuously measuring can not be suitable for measurement vanadium chromium
Vanadium chromium in hydrogen bearing alloy, the problem of measurement result inaccuracy.
The technical solution of present invention solution above-mentioned technical problem are as follows: a kind of company of vanadium chromium content in vanadium chromium hydrogen bearing alloy is provided
Continuous measuring method.Method includes the following steps:
A, vanadium chromium hydrogen bearing alloy sample is weighed, sulfuric acid, phosphoric acid and nitric acid is added and decomposes, vanadium indicator is added, sulfuric acid is added dropwise
Ferrous ammonium salt solution to solution is in bright green, adds liquor potassic permanganate to solution in stable red；
B, urea is added, adds sodium nitrite to solution is red and has just taken off rear excessive 4~5ml, vanadium indicator is added, uses
The titration of iron ammonium sulfate standard solution, when solution becomes bright green from claret, the iron ammonium sulfate standard for recording consumption is molten
The volume of liquid is V1, content of vanadium is calculated；
C, continue to heat solution and boil, silver nitrate solution is added, ammonium persulfate solution is added dropwise to molten in solution fluidized state
Liquid takes on a red color, and continues slightly boiled 5 minutes, and hydrochloric acid solution to red is added dropwise and disappears, then boils and removes cooling, with iron ammonium sulfate standard
Solution is titrated to solution in faint yellow, and vanadium indicator is added dropwise, and continues to be titrated to solution and becomes bright green, record consumption by celadon
Iron ammonium sulfate standard solution volume V2, chromium content is calculated.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, sulfuric acid described in step a is 1+1
Sulfuric acid, the phosphoric acid are to analyze pure, described nitric acid as 1+1 nitric acid.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, urea additional amount described in step b
For 1.4~2.0g is added in every 0.1000 gram of sample.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, the vanadium indicator is N- benzene
Base ortho-aminobenzoic acid.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, the l ferrous ammonium sulfate solution
Concentration is 50~100g/L.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, the calculating of content of vanadium is public in step b
Formula are as follows:M is sample quality g, and C is the concentration mol/L of iron ammonium sulfate standard solution,
V1For the volume mL of iron ammonium sulfate standard solution.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, silver nitrate solution described in step c is dense
Degree is 0.1mol/L, and additional amount is 2.5~3mL.
Wherein, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, the calculating of chromium content is public in step c
Formula are as follows:M is sample quality g, and C is the concentration mol/ of iron ammonium sulfate standard solution
L。
Specifically, in above-mentioned vanadium chromium hydrogen bearing alloy in the method for continuously measuring of vanadium chromium content, comprising the following steps:
A, decomposition samples
Mg vanadium chromium hydrogen bearing alloy sample is weighed, 10~20mL of 1+1 sulfuric acid is added, analyzes 3~5mL of pure phosphoric acid, first heating 3~
5min reheats dissolved samples, and 5~10mL of 1+1 nitric acid is added dropwise to sample and emits homogeneous atmosphere bubble, continues to be heated to just to have emitted white sulphur
Acid fume is cooled to room temperature, and is diluted with water to 80~100mL of volume, and it is limpid to be heated to solution, is removed and is cooled to room temperature；
B, prepare liquid is restored
1 drop vanadium indicator is added dropwise in the solution cooling to step a, 50~100g/L l ferrous ammonium sulfate solution is added dropwise to solution
In bright green, 3~5min is placed；
C, prepare liquid is aoxidized
Liquor potassic permanganate to the solution that 200g/L is added into step b acquired solution is in stable red, excess 1~2
Drop places 2~3min；
D, vanadium measurement interference is eliminated
1.4~2.0g urea is added into step c acquired solution, 10g/L sodium nitrite is added and has just been taken off to solution is red,
Excessive 4~5mL, places 1~2min；
E, vanadium is measured
The vanadium indicator of 2~3 drop 2g/L is added into step d acquired solution, claret occurs to solution, is C with concentration
Iron ammonium sulfate standard solution titration, solution from claret become bright green stop titration, write down consumed iron ammonium sulfate
The volume of standard solution is V1mL；M is sample quality g, and C is iron ammonium sulfate standard
The concentration mol/L, V of solution1For the volume mL of iron ammonium sulfate standard solution.
F, vanadium oxide chromium
The heating of step e acquired solution is boiled, silver nitrate solution is added, the ammonium persulfate solution that 200g/L is added dropwise extremely occurs
Red continues heating and keeps slightly boiled, and the hydrochloric acid solution that 1+3 is added dropwise takes off to red boils 0.5~1min again, removes cooling；
G, vanadium chromium resultant is measured
The iron ammonium sulfate standard solution that step f acquired solution is C with concentration is titrated to faint yellow, 2~3 drop of dropwise addition
The vanadium indicator of 2g/L, continuing to be titrated to solution from celadon becomes bright green, stops titration, writes down consumed iron ammonium sulfate
The volume of standard solution is V2mL；M is sample quality g, and C is iron ammonium sulfate mark
The concentration mol/L of quasi- solution.
Compared with prior art, the invention has the benefit that
Initiative of the invention devises a kind of method for continuously measuring for vanadium high chrome contents high in alloy, widens
The scope of application of vanadium, chromium mark feed method can be suitable for the high vanadium chromium hydrogen bearing alloy of vanadium, chromium content.Also, measurement of the invention
Method avoids the harm to human body and environment without using sodium arsenite poisonous drugs；The present invention can be with using vanadium indicator
Convenient and efficient relatively to accurately control iron ammonium sulfate reduction prepare liquid additional amount, ammonium persulfate solution is added in solution boil condition,
Also it can promptly and accurately judge most economical additional amount, by above-mentioned measure, make measuring method of the present invention accurate and reliable jointly,
It is suitable for promoting the use of.
Specific embodiment
The present invention provides a kind of method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy, comprising the following steps:
A, decomposition samples
M g vanadium chromium hydrogen bearing alloy sample is weighed, 10~20mL of 1+1 sulfuric acid, analysis 3~5mL of pure phosphoric acid is added, first heats 3
~5min reheats dissolved samples, and 5~10mL of 1+1 nitric acid is added dropwise to sample and emits homogeneous atmosphere bubble, continues to be heated to rigid Mao Baise
Sulfuric acid cigarette, is cooled to room temperature, and is diluted with water to 80~100ml of volume, and it is limpid to be heated to solution, removes and is cooled to room temperature；
B, prepare liquid is restored
1 drop vanadium indicator is added dropwise in the solution cooling to step a, 50~100g/L l ferrous ammonium sulfate solution is added dropwise to solution
In bright green, 3~5min is placed；
C, prepare liquid is aoxidized
Liquor potassic permanganate to the solution that 200g/L is added into step b acquired solution is in stable red, excess 1~2
Drop places 2~3min；
D, vanadium measurement interference is eliminated
1.4~2.0g urea is added into step c acquired solution, 10g/L sodium nitrite is added and has just been taken off to solution is red,
Excessive 4~5mL, places 1~2min；
E, vanadium is measured
The vanadium indicator of 2~3 drop 2g/L is added into step d acquired solution, claret occurs to solution, is C with concentration
Iron ammonium sulfate standard solution titration, solution from claret become bright green stop titration, write down consumed iron ammonium sulfate
The volume of standard solution is V1mL；M is sample quality g, and C is that iron ammonium sulfate standard is molten
The concentration mol/L, V of liquid1For the volume mL of iron ammonium sulfate standard solution.
F, vanadium oxide chromium
The heating of step e acquired solution is boiled, silver nitrate solution is added, the ammonium persulfate solution that 200g/L is added dropwise extremely occurs
Red continues heating and keeps slightly boiled, and the hydrochloric acid solution that 1+3 is added dropwise takes off to red boils 0.5~1min again, removes cooling；
G, vanadium chromium resultant is measured
The iron ammonium sulfate standard solution that step f acquired solution is C with concentration is titrated to faint yellow, 2~3 drop of dropwise addition
The vanadium indicator of 2g/L, continuing to be titrated to solution from celadon becomes bright green, stops titration, writes down consumed iron ammonium sulfate
The volume of standard solution is V2mL；M is sample quality g, and C is iron ammonium sulfate mark
The concentration mol/L of quasi- solution.
In the above method, 1 drop vanadium indicator is added dropwise in step b, is titrated to solution with 50~100g/L l ferrous ammonium sulfate solution
In bright green.The purpose that vanadium indicator is added dropwise is to judge vanadium chromium reducing degree by color change, is adjusted to solution in bright green
Operation do not need too accurate, as long as excessive 1~2 drop will not influence subsequent operations, indicate if not having to indicator, be arbitrarily added
L ferrous ammonium sulfate solution in most cases all can be excessive, increases to will lead to subsequent potassium permanganate oxidation dosage, increase at
This.
In the above method, 1.4~2.0g urea is added in step d solution, has just been taken off with 10g/L sodium nitrite reduction red,
Excessive 4~5mL, is placed 1~2 minute；It is slightly more compared to existing method amount of urea, it, cannot such as amount of urea deficiency
Excessive sodium nitrite is all decomposed, the vanadium of part can be restored, keep vanadium measurement result relatively low.Excessively 4~5mL is sodium nitrite
Also the reaction of postorder ferrous iron solution can be participated in by being oxidized to eliminate high chrome contents a small amount of chromium during potassium permanganate oxidation, amount
Deficiency cannot completely eliminate the interference of chromium, place certain time be since the reaction of chromium and sodium nitrite needs certain time, it is molten
There are certain sodium nitrites can decompose vanadium indicator in liquid, influences to develop the color, and places certain time also for ensuring excessive nitrous
Sour sodium can be reacted completely by urea.
In the above method, the solution heating of step f is boiled, a certain amount of silver nitrate solution is added, a certain amount of 200g/L's
Ammonium persulfate solution continues heating and keeps slightly boiled certain time, hydrochloric acid solution to the red that 1+3 is added dropwise is taken off again to there is red
It boils 0.5~1 minute, removes cooling, wherein the concentration of silver nitrate is 0.1mol/L, is approximately equal to the aqueous solution of 17g/L, additional amount
For 2.5~3mL, if additional amount is very little, add ammonium persulfate amount is more to be again also difficult that (solution is not in by whole vanadium and chromium oxidation
It is red), under the premise of ensuring silver nitrate dosage, the dosage of ammonium persulfate is depending on vanadium chromium content in sample, and dosage is to ensure
It is principle that vanadium and chromium, which are all oxidizing to highest price and need not excessively cause waste too much, concrete operation method: solution is kept to boil
Ammonium persulfate solution is added dropwise with dropper under state, red occurs in solution, is 50%~65% by content of vanadium in sample, chromium contains
Amount is 10%~25% ammonium persulfate solution for taking around 200g/L in 15~35mL range, is equivalent to 3~7 grams of solid over cures
Sour ammonium.
A specific embodiment of the invention is further explained below with reference to embodiment and screening experiment, but not
Protection scope of the present invention is limited in range described in embodiment by expression.
Used main agents and simulant standard samples are as follows in embodiment and screening experiment:
(1) vanadium standard liquid (2mg/mL): 2.0000g metal vanadium powder is accurately weighed in 500mL conical flask, distilled water is added to moisten
It is wet, (1+1) sulfuric acid 50mL is added, dissolves by heating, nitric acid (1+1) about 20mL is added dropwise during heating, is heated to emitting sulfuric acid cigarette,
Cooling is removed, 50mL distilled water is added, is cooled to room temperature, is moved into 1000mL volumetric flask, constant volume shakes up.
(2) chromium standard liquid (1mg/mL): 1.0000g hafnium metal powfer is accurately weighed in 500mL conical flask, distilled water is added to moisten
It is wet, (1+1) sulfuric acid 50mL is added, dissolves by heating, nitric acid (1+1) about 20mL is added dropwise during heating, is heated to emitting sulfuric acid cigarette,
Cooling is removed, 50mL distilled water is added, is cooled to room temperature, is moved into 1000mL volumetric flask, constant volume shakes up.
(3) silica 3.0003g, metal vanadium powder 11.9998g, hafnium metal powfer 2.5001g, three oxygen simulant standard samples: are weighed
Change two iron 0.8005g, aluminum oxide 2.0002g, be uniformly mixed to obtain simulant standard samples, wherein shared content is vanadium in the sample
59.11%, shared content is 12.32% to chromium in the sample.
(4) silver nitrate solution (0.1mol/L) aqueous solution；
(5) ammonium persulfate solution (200g/L) aqueous solution；
(6) urea liquid 200g/L aqueous solution.
Screening experiment 1: the influence that amount of urea measures content of vanadium
To weigh 0.1000 gram of sample, chromium content is between 10~25%, the chromium content being converted into sample, divides and takes chromium standard liquid
Amount, pipettes more parts of chromium standard liquid (1mg/mL) 10,20mL respectively, pipettes more parts of 25mL of vanadium standard liquid (2mg/mL), excessive 10g/L nitrous
The volume of sour sodium is 5mL, only changes the dosage of urea, other steps are carried out by the method provided in previous embodiment
Time-and-motion study vanadium amount is carried out calculating to obtain content of vanadium by 0.1000g sample weighting amount, and acquired results are shown in Table 1.
1 amount of urea of table tests (urea concentration: 200g/L)
It was found from 1 data of table: when amount of urea deficiency, measurement vanadium amount is relatively low, which is because, excessive sodium nitrite does not have
Having enough urea to decompose can react with a small amount of high price vanadium, and with the increase of chromium content in sample, excessive sodium nitrite is added
When enough, urea amount used can be reduced, and for vanadium chromium hydrogen bearing alloy, excessive 10g/L sodium nitrite 5mL is added
7~10mL of urea liquid of 200g/L is equivalent to 1.4~2.0 grams of solid urea.In addition, it is molten that excessive nitrite sodium is added
Placement is had to after liquid 1~2 minute just be added vanadium indicator titrated, otherwise there is excessive sodium nitrite to vanadium indicator
There is decomposition, the not aobvious color of solution or color are very shallow, influence endpoint.
Screening experiment 2: influence of the silver nitrate dosage to chromium content
It finds in the course of the research, how much silver nitrate dosage determines whether vanadium chromium resultant can be completely oxidized to most in sample
The key of high price, dosage is insufficient, adds ammonium persulfates more again that whole vanadium can not be oxidized to 5 valences and whole chromium and is oxidized to
6 valences, silver nitrate are a kind of more expensive chemical reagent, and dosage is too many, increase cost, therefore, use of the present invention to silver nitrate
Amount has carried out following screening.
Equally tested using vanadium and chromium standard liquid: according to 0.1000 gram of sample weighting amount, chromium content is between 10~25%, folding
The chromium content in sample is calculated, divides and takes chromium standard liquid amount, pipette more parts of chromium standard liquid (1mg/mL) 10,20mL respectively, pipette vanadium standard liquid
The volume of more parts of (2mg/mL) 25mL, excessive 10g/L sodium nitrite are 5mL, and 200g/L urea liquid 8mL is added, and measure vanadium
Afterwards, silver nitrate solution (0.1mol/L) not same amount, addition ammonium persulfate solution (200g/L) 35mL is added, before other steps are pressed
The method provided in mask body embodiment carries out time-and-motion study vanadium chromium resultant, carries out calculating chromium content, institute by 0.1000g sample weighting amount
2 must be the results are shown in Table.
2 silver nitrate dosage of table tests (silver nitrate solution concentration: 0.1mol/L)
In the case where guaranteeing the enough situations of ammonium persulfate dosage, silver nitrate dosage is to determine vanadium and the whether whole oxygen of chromium in solution
The key of change can be oxidized to red from solution to judge whether vanadium and chromium are completely oxidized to high price, and solution is boiling
As long as with the presence of the chromium of low price under state, there will be no the red of MnO4 to occur, as long as therefore having manganese ion to deposit in solution
, so that it may by occurring MnO4 red, the judgment basis being all oxidized as vanadium in solution and chromium in solution.Solution
Subsequent operations cannot be carried out by not occurring red.As can be known from Table 2: in the identical situation of ammonium persulfate dosage, silver nitrate
Dosage is insufficient, vanadium and chromium cannot be completely oxidized to high price, when 1mL is added in silver nitrate, solution colour is still in that yellow shows greatly
The vanadium and chromium of amount are oxidized to high price, and when 2mL is added in silver nitrate, solution colour shows vanadium and chromium close to all by oxygen in yellowish-brown
MnO4 red will occur in chemical conversion high price, when 2.5~3mL is added in silver nitrate, solution colour takes on a red color, and shows vanadium and chromium
It has all been oxidized to high price, MnO4 red has occurred, can also find out from table 2, chromium content height phenomenon is all essentially the same, real
Test the result shows that: silver nitrate dosage can ensure that in solution that vanadium and chromium are all oxidized to high price in 2.5~3mL, measurement result and
Standard value is coincide preferable.
Vanadium chromium METHOD FOR CONTINUOUS DETERMINATION in embodiment hydrogen bearing alloy
Vanadium in vanadium chromium hydrogen bearing alloy sample and simulant standard samples and chromium are determined as follows, specific method is such as
Under:
(1) sample decomposes: weighing about 0.1000 gram of sample and simulant standard samples, is put in the triangular flask of 500mL, (1+ is added
1) sulfuric acid 20mL, analysis pure phosphoric acid 3mL, are first heated 3~5 minutes on low-temperature furnace, then examination is dissolved by heating on high-temperature electric resistance furnace
Sample is added dropwise 1+1 nitric acid oxidation and sample is promoted to decompose, until sample emits homogeneous atmosphere bubble, consumes about 5~10mL, continues to heat
It to white sulfuric acid cigarette is just emitted, removes and is cooled to room temperature, be diluted with water to volume about 100mL, it is limpid to be heated to solution, removes cooling
To room temperature；
(2) it measures vanadium: adding 1 drop vanadium indicator, be adjusted to solution with 100g/L l ferrous ammonium sulfate solution is become from yellow green
Bright green, then dripped with the potassium permanganate oxidation of 20g/L to red appearance excessive 1~2 is stablized, it places 2~3 minutes, 200g/ is added
L urea 8mL has just been taken off with 10g/L sodium nitrite reduction red, and excessive 5mL is placed 1~2 minute, and 3 drop 2g/L vanadium instructions are added dropwise
Agent is in claret (about 10 seconds) to solution, and being titrated to solution with iron ammonium sulfate standard solution becomes dark brown from claret
Becoming bright green again is that vanadium measures terminal, writes down consumption iron ammonium sulfate standard solution volume V1；
(3) it measures chromium: 0.1mol/L silver nitrate solution 3mL is added to the solution after measurement vanadium, heats and is dripped under boil condition
Add the ammonium persulfate solution of 200g/L until solution occurs red (about 20~25mL), continues heating and keep slightly boiled 5
Minute, the hydrochloric acid solution that 1+3 is added dropwise disappears (about 2mL) to red, then boils, and removes and is cooled to room temperature, uses iron ammonium sulfate
Standard solution is titrated to faint yellow, 3 drop vanadium indicator is added dropwise, continuing to be titrated to celadon and becoming bright green is that vanadium chromium resultant titrates
Terminal writes down consumption iron ammonium sulfate standard solution volume V2；
(4) data are handled by vanadium and chromium calculating formula, acquired results are shown in Table 3.
Vanadium chromium METHOD FOR CONTINUOUS DETERMINATION result in 3 hydrogen bearing alloy of table
To find out from 3 result of table, the method for the present invention is all higher to the preci-sion and accuracy of the measurement of vanadium chromium in hydrogen bearing alloy,
All in allowable error range, show that the invention patent implementation result is good.
Claims (9)
1. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy, which comprises the following steps:
A, vanadium chromium hydrogen bearing alloy sample is weighed, sulfuric acid, phosphoric acid and nitric acid is added and decomposes, vanadium indicator is added, ferrous sulfate is added dropwise
Ammonium salt solution to solution is in bright green, adds liquor potassic permanganate to solution in stable red；
B, urea is added, adds sodium nitrite to solution is red and has just taken off rear excessive 4~5mL, vanadium indicator is added, uses sulfuric acid
The titration of ferrous ammonium standard solution, when solution becomes bright green from claret, records the iron ammonium sulfate standard solution of consumption
Volume is V1, content of vanadium is calculated；
C, continue to heat solution and boil, silver nitrate solution is added, solution fluidized state is added dropwise ammonium persulfate solution to solution and is in
Red continues slightly boiled 5 minutes, and hydrochloric acid solution to red is added dropwise and disappears, then boils and removes cooling, with iron ammonium sulfate standard solution
Solution is titrated in faint yellow, vanadium indicator is added dropwise, continues to be titrated to solution bright green is become by celadon, records the sulphur of consumption
Sour ferrous ammonium standard solution volume V2, chromium content is calculated.
2. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: step
Sulfuric acid described in a is 1+1 sulfuric acid, and the phosphoric acid is to analyze pure, described nitric acid as 1+1 nitric acid.
3. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: step
Urea additional amount described in b is that 1.4~2.0g is added in every 0.1000 gram of sample.
4. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: described
Vanadium indicator be N- phenylanthranilic acid.
5. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: described
L ferrous ammonium sulfate solution concentration be 50~100g/L.
6. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: step
The calculation formula of content of vanadium in b are as follows:M is sample quality g, and C is iron ammonium sulfate standard
The concentration mol/L, V of solution1For the volume mL of iron ammonium sulfate standard solution.
7. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: step
Silver nitrate solution concentration described in c is 0.1mol/L, and additional amount is 2.5~3mL.
8. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, it is characterised in that: step
The calculation formula of chromium content in c are as follows:M is sample quality g, and C is iron ammonium sulfate
The concentration mol/L of standard solution.
9. the method for continuously measuring of vanadium chromium content in vanadium chromium hydrogen bearing alloy according to claim 1, which is characterized in that including
Following steps:
A, decomposition samples
Mg vanadium chromium hydrogen bearing alloy sample is weighed, 10~20mL of 1+1 sulfuric acid is added, analyzes 3~5mL of pure phosphoric acid, first heating 3~
5min reheats dissolved samples, and 5~10mL of 1+1 nitric acid is added dropwise to sample and emits homogeneous atmosphere bubble, continues to be heated to just to have emitted white sulphur
Acid fume is cooled to room temperature, and is diluted with water to 80~100mL of volume, and it is limpid to be heated to solution, is removed and is cooled to room temperature；
B, prepare liquid is restored
1 drop vanadium indicator is added dropwise in the solution cooling to step a, 50~100g/L l ferrous ammonium sulfate solution is added dropwise to solution in bright
Green places 3~5min；
C, prepare liquid is aoxidized
Liquor potassic permanganate to the solution that 200g/L is added into step b acquired solution is in stable red, and excessive 1~2 drips, and is put
Set 2~3min；
D, vanadium measurement interference is eliminated
1.4~2.0g urea is added into step c acquired solution, 10g/L sodium nitrite is added and has just been taken off to solution is red, it is excessive
4~5mL places 1~2min；
E, vanadium is measured
The vanadium indicator of 2~3 drop 2g/L is added into step d acquired solution, claret occurs to solution, the sulphur for being C with concentration
Sour ferrous ammonium standard solution titration, solution become bright green from claret and stop titration, write down consumed iron ammonium sulfate standard
The volume of solution is V1mL；M is sample quality g, and C is iron ammonium sulfate standard solution
Concentration mol/L, V1For the volume mL of iron ammonium sulfate standard solution.
F, vanadium oxide chromium
The heating of step e acquired solution is boiled, silver nitrate solution is added, the ammonium persulfate solution that 200g/L is added dropwise is red to occurring
Color continues heating and keeps slightly boiled, and the hydrochloric acid solution that 1+3 is added dropwise takes off to red boils 0.5~1min again, removes cooling；
G, vanadium chromium resultant is measured
The iron ammonium sulfate standard solution that step f acquired solution is C with concentration is titrated to faint yellow, 2~3 drop 2g/L are added dropwise
Vanadium indicator, continuing to be titrated to solution from celadon becomes bright green, stops titration, it is molten to write down consumed iron ammonium sulfate standard
The volume of liquid is V2mL；M is sample quality g, and C is iron ammonium sulfate standard solution
Concentration mol/L.
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| CN111257503A (en) * | 2020-04-01 | 2020-06-09 | 李岩 | Method for detecting chromium content of high-chromium-content aluminum alloy based on titration analysis method |
| CN113588868A (en) * | 2021-09-15 | 2021-11-02 | 中冶北方（大连）工程技术有限公司 | Method for measuring chromium content in chromium ore by ammonium ferrous sulfate volumetric method |
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| CN113588868A (en) * | 2021-09-15 | 2021-11-02 | 中冶北方（大连）工程技术有限公司 | Method for measuring chromium content in chromium ore by ammonium ferrous sulfate volumetric method |
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