CN108872223A - A kind of method of phosphorus content in measurement molybdenum compound - Google Patents
A kind of method of phosphorus content in measurement molybdenum compound Download PDFInfo
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Abstract
The present invention provides a kind of methods of phosphorus content in measurement molybdenum compound, including：Molybdenum compound sample is decomposed, decomposed solution is obtained；The reagent of the decomposition includes water, perchloric acid and hydrogen peroxide；The decomposed solution is developed the color, developing solution is obtained；The developing solution is tested in the absorbance of 680~700nm wave-length coverage.Compared with prior art, measuring method provided by the invention is during decomposition samples, phosphorus in sample is directly pentavalent phosphorus by hydrogen peroxide oxidation, then phosphorus content is measured by blue spectrophotometry, it is easy to operate, and do not use poisonous substance during whole operation and generate toxic gas, it is very environmentally friendly, and the interference of silicon is not present, test result is accurate.The method of phosphorus content is easy to operate, quick, environmentally friendly in measurement molybdenum compound provided by the invention, and testing result is accurate, the phosphorus content being particularly suitable in detection molybdenum-iron or metal molybdenum.
Description
Technical field
The present invention relates to phosphorus contents in molybdenum compound chemical analysis technology field more particularly to a kind of measurement molybdenum compound
Method.
Background technique
Currently, the method for phosphorus content is broadly divided into two classes in measurement molybdenum-iron, one kind is using dust technology decomposition samples, with height
Phosphorus oxygen is turned to pentavalent phosphorus by potassium manganate, then using blue spectrophotometry measurement.Another kind of is to mix molybdenum-iron sample with nitrate
After closing acid decomposition, addition perchloric acid heating emits perchloric acid cigarette and phosphorus oxygen is turned to pentavalent phosphorus, then is measured with blue light light indexing.It is existing
After these two types of detection method decomposition samples that technology provides, it is complex that phosphoric step is converted by the phosphorus in sample, the
A kind of method uses toxic potassium permanganate, decomposes manganese dioxide precipitate object and uses toxic sodium nitrite, generates toxic nitrogen
Oxide gas, and the result of the silicon severe jamming detection in sample.Second class method generates toxic perchloric acid cigarette.
The method consumption reagent of phosphorus content is more, complicated for operation in the detection molybdenum-iron that the prior art provides, and not environmentally.Cause
This, providing the method that one kind preferably detects phosphorus content in molybdenum compound becomes those skilled in the art's urgent problem to be solved.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of method of phosphorus content in measurement molybdenum compound, the present invention is mentioned
The measuring method simple process of confession, consumption reagent are few, safety and environmental protection, and testing result accuracy is high.
The present invention provides a kind of methods of phosphorus content in measurement molybdenum compound, including：
Molybdenum compound sample is decomposed, decomposed solution is obtained；The reagent of the decomposition includes water, perchloric acid and hydrogen peroxide；
The decomposed solution is developed the color, developing solution is obtained；
The developing solution is tested in the absorbance of 680~700nm wavelength.
The present invention does not have special limitation to the type of the molybdenum compound and source, using known to those skilled in the art
Molybdenum compound, can by market buy obtain.In the present invention, the molybdenum compound can may be metal for molybdenum-iron
Molybdenum, preferably molybdenum-iron.In the present invention, the molybdenum-iron is preferably standard molybdenum-iron substance, as GSB03-1563-2003 molybdenum-iron,
YSBC37653-10 molybdenum-iron, BH0314-4 molybdenum-iron, YSBC18605-08 molybdenum-iron, GSB03-1689-2004 molybdenum-iron, GSBC2013-
57 molybdenum-irons or YSBC37653-10 molybdenum-iron.
In the present invention, the mass content of phosphorus is preferably 0.01~0.5% in the molybdenum compound, more preferably 0.05~
0.4%, more preferably 0.1~0.3%, most preferably 0.15~0.25%.
The present invention does not have special limitation to the preparation method of the molybdenum compound sample, ripe according to those skilled in the art
Prepared by the method for making sample for the test button for composition detection known, such as can refer to GB/T 20066《Steel and iron
Study sampling and the method for making sample of point measurement sample》Molybdenum compound sample is prepared in method for making sample provided in standard.
In the present invention, reagent used is preferably analytically pure reagent, and water used is preferably distilled water or deionization
Water, or the water of purity suitable with its.
In the present invention, the density of the perchloric acid is preferably 1.65~1.75g/mL, more preferably 1.68~1.72g/
ML, most preferably 1.69g/mL.The present invention does not have special limitation to the type of the perchloric acid and source, using this field skill
Perchloric acid known to art personnel can be bought by market and be obtained.
In the present invention, the hydrogen peroxide is preferably hydrogenperoxide steam generator, more preferably aqueous hydrogen peroxide solution.At this
In invention, the mass concentration of the hydrogenperoxide steam generator is preferably 25~35%, and more preferably 28~32%, most preferably
30%.
In the present invention, the volume ratio of the water, hydrogenperoxide steam generator and perchloric acid is preferably 40:(15~25)：(15~
25), more preferably 40:(18~22):(18~22), most preferably 40:20:20.
In the present invention, the dosage of the molybdenum compound sample is preferably 0.2~0.3g, more preferably 0.22~0.28g,
Most preferably 0.24~0.26g.In the present invention, 0.0001g is preferably accurate to during weighing molybdenum compound.In the present invention
In, the usage ratio of the reagent of the molybdenum compound sample and decomposition is preferably (0.2~0.3) g:(70~90) mL, more preferably
For (0.22~0.28) g：(72~78) mL, most preferably (0.24~0.26) g:(74~76) mL.
In the present invention, the method for decomposing molybdenum compound sample is preferably：
Addition perchloric acid mixing is decomposed after water, hydrogenperoxide steam generator mixing are added into molybdenum compound sample, sample
It is heated to vigorous reaction (generating a large amount of bubbles in the short time) after decomposing completely, stops heating, vigorous reaction is (big after stopping
Measure bubble collapse), heating is boiled does not have about 1 millimeter of diameter of minute bubbles to generate into solution, generates about 3~5 millimeters of diameter
Air pocket indicates that hydrogen peroxide decomposes completely, then cools to room temperature, be diluted with water, obtain decomposed solution.
In the present invention, the colour developing is that ingredient to be detected is made to be changed into stable colored compound.In the present invention,
The method of the colour developing is preferably：
The decomposed solution, hypo solution and mixed liquor are mixed, developing solution is obtained；
The mixed liquor includes：Perchloric acid, gum arabic solution, bismuth salt solution, ammonium molybdate solution and ascorbic acid are molten
Liquid.
In the present invention, the decomposed solution is consistent with decomposed solution described in above-mentioned technical proposal, and details are not described herein.
In the present invention, the concentration of the hypo solution is preferably 8~12g/L, more preferably 9~11g/L, most
Preferably 10g/L.In the present invention, the preparation method of the thiosulfuric acid solution is preferably：
Add water after sodium sulfite and sodium thiosulfate are mixed, obtains hypo solution.
In the present invention, since hypo solution is easy oxidation by air, be added has strong go back during the preparation process
The sodium sulfite of originality can prevent hypo solution oxidation by air.
In the present invention, the sodium sulfite is preferably anhydrous sodium sulfite.In the present invention, the sodium sulfite and sulphur
The mass ratio of sodium thiosulfate is preferably (3~7)：1, more preferably (4~6)：1, most preferably 5:1.In the present invention, described mixed
The method of conjunction is preferably stirred to sodium sulfite and sodium thiosulfate and is completely dissolved.
In the present invention, the perchloric acid is consistent with perchloric acid described in above-mentioned technical proposal, and details are not described herein.
In the present invention, the mass concentration of the gum arabic solution is preferably 15~25g/L, more preferably 18~
22g/L, most preferably 20g/L.In the present invention, the gum arabic solution is preferably Arabic gum aqueous solution.This hair
The bright source to the gum arabic solution does not have specific limitation, can be bought and be obtained by market, can also be according to art technology
The preparation method of solution known to personnel is prepared.
In the present invention, the concentration of the bismuth salt solution is preferably 45~55g/L, more preferably 48~52g/L, most preferably
For 50g/L.In the present invention, the bismuth salt solution is the perchloric acid solution of bismuth nitrate.In the present invention, the bismuth salt solution
Preparation method is preferably：
Bismuth nitrate and perchloric acid are mixed.
In the present invention, the usage ratio of the bismuth nitrate and perchloric acid is preferably 1g:(5~15) mL, more preferably 1g:
(8~12) mL, most preferably 1g:10mL.
In the present invention, the mixed method is preferably heating stirring dissolution, and the temperature of the heating is preferably seen
There is smoke event in perchloric acid.In the present invention, it is diluted with water after being preferably cooled to room temperature after the completion of the heating.
In the present invention, the concentration of the ammonium molybdate solution is preferably 45~55g/L, more preferably 48~52g/L, optimal
It is selected as 50g/L.In the present invention, the preparation method of the ammonium molybdate solution is preferably：
Ammonium molybdate and water are mixed, ammonium molybdate solution is obtained.
In the present invention, the mixed method preferably dissolves by heating, and the temperature of the heating preferably makes ammonium molybdate
It is completely dissolved；In the present invention, it is diluted with water after being preferably cooled to room temperature after the completion of the heating for dissolving.In the present invention, institute
The usage ratio for stating ammonium molybdate and water is preferably 25g：(450~550) mL, more preferably 25g：(480~520) mL, most preferably
For 25g：480mL.
In the present invention, the concentration of the ascorbic acid solution is preferably 95~105g/L, more preferably 98~102g/L,
Most preferably 100g/L.In the present invention, the ascorbic acid solution is preferably the aqueous solution of ascorbic acid.The present invention is to described
The source of ascorbic acid solution does not have special limitation, can be bought and be obtained by market, can also be according to known to those skilled in the art
The preparation method of ascorbic acid solution be prepared.
In the present invention, the preparation method of the mixed liquor is preferably：
Perchloric acid, bismuth salt solution and gum arabic solution are mixed, the first mixture is obtained；
First mixture and ammonium molybdate solution are mixed, the second mixture is obtained；
Second mixture and ascorbic acid solution are mixed, mixed liquor is obtained.
In the present invention, the perchloric acid, bismuth salt solution, gum arabic solution, ammonium molybdate solution and ascorbic acid are molten
Perchloric acid described in type, source and the concentration and above-mentioned technical proposal of liquid, bismuth salt solution, gum arabic solution, ammonium molybdate are molten
Liquid and the type of ascorbic acid solution, source are consistent with concentration, and details are not described herein.
In the present invention, the perchloric acid, bismuth salt solution, gum arabic solution, ammonium molybdate solution and ascorbic acid are molten
The volume ratio of liquid is preferably 100:(25~45):(95~105):(95~105):(55~65), more preferably 100:(28~
42):(98~102):(98~102):(58~62), most preferably 100:40:100:100:60.
In the present invention, the volume ratio of the decomposed solution, hypo solution and mixed liquor is preferably (5~20)：(3
~7)：(15~25), more preferably (10~15)：(4~6)：(18~22), most preferably (12~13)：5：20.
In the present invention, it obtains the present invention after developing solution and the developing solution is preferably taken to the test for carrying out absorbance after liquid.
In the present invention, in molybdenum compound sample phosphorus mass content≤0.1% when, liquid-taken amount is preferably 15~25mL, more preferably
18~22mL, most preferably 20mL；When the mass content of phosphorus is 0.1~0.2% in molybdenum compound sample, liquid-taken amount is preferably 5
~15mL, more preferably 8~12mL, most preferably 10mL；When the mass content of phosphorus is 0.2~0.4% in molybdenum compound sample,
Sampling amount is preferably 3~7mL, more preferably 4~6mL, most preferably 5mL.
The present invention does not have special limitation in the test method of the absorbance of 680~700nm wavelength to the developing solution, adopts
It is tested with the test method of test specific wavelength absorbance well known to those skilled in the art, such as can refer to GB
7729《Metallurgic product chemical analysis method spectrophotometry general rule》It is detected.In the present invention, the test of the absorbance
It is preferred that being tested using visible light photometer, the present invention does not have special limit to the photometric type of the visible light and source
System, is tested using visible light photometer well known to those skilled in the art, can be bought and be obtained by market, according to being made
The photometric operation instruction of visible light is tested.In the present invention, the visible light photometer is preferably 722 types
Visible light photometer.
In the present invention, the developing solution is in the test process of the absorbance of 680~700nm wavelength, reference used
Sample does not weigh molybdenum-iron sample preferably, and weighs high purity iron, the preferred < 0.001% of the mass content of phosphorus in the high purity iron；
The dosage of high-purity ferroelectric sample is preferably 0.1g.
In the present invention, to the developing solution before the absorbance of 680~700nm wavelength is tested, preferably by institute
Developing solution is stated to place at room temperature.In the present invention, the temperature of the room temperature is preferably 20~30 DEG C, more preferably 22~28
DEG C, most preferably 24~26 DEG C；The time of the placement is preferably 20~30 minutes, and more preferably 22~28 minutes, most preferably
It is 24~26 minutes.In the present invention, the wavelength during absorbance detection is preferably 680~700nm, more preferably 685~
695nm, most preferably 690nm.
In the present invention, it after obtaining absorbance, is preferably obtained from working curve function according to the numerical value of absorbance corresponding
Phosphorus quality, the working curve function be known standard sample in phosphorus quality and absorbance corresponding relationship function.The present invention
There is no special limitation to the preparation method of the working curve function, using working curve letter well known to those skilled in the art
Several preparation methods obtains, i.e., is carried out according to the method provided by the invention using a series of standard sample of known phosphorus quality
The corresponding relationship curve of phosphorus quality and absorbance is established in the test of absorbance, is carried out linear fit to the curve, is obtained work
Function curve.
In the present invention, the preparation method of the working curve function is preferably：
A series of different standard sample sample of 5~6 parts of phosphorus contents is weighed, the phosphorus content range for controlling standard sample includes
The phosphorus content of sample to be tested, the phosphorus content of the standard sample ranges preferably from 0.01~0.5%, more preferably 0.05~
0.4%, more preferably 0.1~0.3%, most preferably 0.15~0.25%.
According to operating procedure same as phosphorus content in said determination molybdenum compound, test obtains the molybdenum of serial phosphorus content
The absorbance for closing object, acquires working curve function for phosphorus content progress linear regression corresponding with absorbance.
In the present invention, the mass content for calculating phosphorus in molybdenum compound after working curve function according to the following equation is obtained：
Wherein, m1Quality for the phosphorus checked on working curve, g；
m0For the quality of sample, g.
The present invention decomposes molybdenum compound sample using the mixed liquor of water, perchloric acid and hydrogen peroxide, molten with sodium thiosulfate
Liquid shelters arsenic, and the arsenic in sodium thiosulfate and solution forms stable compound, arsenic is made not re-form arsenic molybdenum in the follow-up process
Heteropoly compound measures phosphorus content with blue light degree indexing.
Compared with prior art, measuring method provided by the invention, during decomposition samples, the phosphorus in sample is direct
It is pentavalent phosphorus by hydrogen peroxide oxidation, phosphorus content is then measured by the blue light degree indexing of dilute perchloric acid medium, it is easy to operate,
And do not use poisonous substance during whole operation and generate toxic gas, it is very environmentally friendly, and the interference of silicon is not present,
Test result is accurate.The method of phosphorus content is easy to operate, quick, environmentally friendly in measurement molybdenum-iron provided by the invention, and testing result is quasi-
Really, the phosphorus content being particularly suitable in detection molybdenum-iron or metal molybdenum.
It is easy to operate the present invention provides a kind of blue light degree indexing of phosphorus content in novel Accurate Determining molybdenum compound,
Environmental protection, the repeatability and repdocutbility of testing result are preferable.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff it is improved or retouching all other example, shall fall within the protection scope of the present invention.
Raw materials used following embodiment of the present invention is commercial goods.
Embodiment 1 detects phosphorus content in GSB03-1563-2003 standard molybdenum-iron
(1) sample preparation is taken
According to GB/T 20066-2006《The sampling of steel and iron chemical composition sample and method for making sample》Standard pair
GSB03-1563-2003 standard sample is sampled.
(2) sample weighting amount
Sample 0.25g is weighed, 0.0001g is accurate to.
Reagent blank (water) is done in company with sample, does not weigh molybdenum-iron sample, and weighs 0.10g high purity iron (phosphorous quality <
0.001%).
(3) sample dissolves
Sample is placed in 300mL triangular flask or optical port beaker, 40 milliliters of water are added, 20 milliliters of mass concentrations, which are added, is
30% hydrogenperoxide steam generator mixes, and 20 milliliters of perchloric acid (density 1.69g/mL) is added and mixes, sample is completely dissolved
Afterwards, when being heated to the vigorous reaction a large amount of bubbles of generation, stop heating, after vigorous reaction stops, heating is boiled not to be had into solution
The minute bubbles of diameter about 1mm and after generating the air pocket that diameter is 3~5mm, cooling room temperature, being diluted with water is 100.00 milliliters,
It mixes, obtains mother liquor.
(4) mother liquor is pipetted
Mother liquor 20mL is pipetted in 50 milliliters of volumetric flask.
(5) it develops the color
The concentration that 5mL is added into above-mentioned mother liquor is the hypo solution of 10g/L, mixes, the mixing of 20mL is added
Liquid mixes, is diluted with water to 50mL, obtains developing solution.
The preparation method of the mixed liquor is：
In the wide mouth beaker of 1000mL, 100 milliliters of perchloric acid (density 1.69g/mL) is added, is added 40 milliliters
The gum arabic solution (20g/L) of 100mL is added in bismuth salt solution, mixes, and 100 milliliters of ammonium molybdate solution (50g/ is added
L), mix, the ascorbic acid solution (100g/L) of 60mL is added with the mode being added while stirring, mix, obtain mixed liquor.
The preparation method of the bismuth salt solution is：
It takes the bismuth nitrate of 50.0g in the wide mouth beaker of 100mL, the perchloric acid (density 1.67g/mL) of 500mL is added,
Heating stirring dissolution is complete and is heated to seeing that perchloric acid cigarette is emerged, and is cooled to room temperature, and being diluted with water is 1000 milliliters, mixes.
The preparation method of the ammonium molybdate solution is：
It is weighed into the ammonium molybdate of 25.0g in the wide mouth beaker of 600mL, 400 milliliters of water is added, dissolves by heating completely, it is cold
But to room temperature, being diluted with water is 500 milliliters, is mixed.
The preparation method of the hypo solution is：
50g anhydrous sodium sulfite and 10.0g sodium thiosulfate are weighed in 1000 milliliters of wide mouth beakers, adding water to solution is
1000 milliliters, stirring to anhydrous sodium sulfate and sodium thiosulfate dissolution are complete.
(6) absorbance is measured
In on 722 type visible spectrophotometers after above-mentioned developing solution is placed at room temperature for 25 minutes, appropriately sized suction is chosen
It receives ware and at 690nm wavelength, tests the absorbance of developing solution using water as reference.
(7) test job curvilinear function
Take the standard molybdenum-iron sample specimens that a series of 5 parts of phosphorus contents are different, the phosphorus content model of 5 parts of standard molybdenum-iron sample specimens
The phosphorus content including sample to be tested is enclosed, is operated according to above-mentioned steps (1)~(6), test obtains 5 parts of different phosphorus content standards
The absorbance of molybdenum-iron sample, the phosphorus content of standard sample is carried out with the data of absorbance corresponding, and drafting obtains working curve, right
Curve carries out linear regression, acquires working curve function.
(8) it calculates
The mass content of phosphorus in molybdenum-iron to be measured is calculated according to the following equation：
In formula, m1To bring the absorbance of sample to be tested into the phosphorus quality that working curve function is calculated, g；
m0For sample to be tested quality, g.
According to the method described above, sample to be tested is detected twice, the result detected twice is that phosphorus mass content is
0.0325% and 0.0321%, the standard value of the mass content of phosphorus is in standard sample to be measured used in the present embodiment
0.032%, tolerance 0.004%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is to phosphorus content
Testing result is accurate, and repeatability and repdocutbility are preferable.
Embodiment 2 detects phosphorus content in YSBC37653-2010 standard molybdenum-iron
It is detected according to method described in embodiment 1, testing result is that phosphorus mass content is in sample to be tested
0.0455%, the standard value of the mass content of phosphorus is 0.046% in standard sample to be measured used in the present embodiment, and tolerance is
0.004%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is accurate to the testing result of phosphorus content.
Embodiment 3 detects phosphorus content in BH0314-4 standard molybdenum-iron
It is detected according to method described in embodiment 1, testing result is that phosphorus mass content is in sample to be tested
0.0218%, the standard value of the mass content of phosphorus is 0.023% in standard sample to be measured used in the present embodiment, and tolerance is
0.0025%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is accurate to the testing result of phosphorus content.
Embodiment 4 detects phosphorus content in YSBC18605-08 standard molybdenum-iron
3 detections are carried out according to method described in embodiment 1, the difference from embodiment 1 is that, the amount for pipetting masterbatch is
10mL。
Testing result is that phosphorus mass content is respectively 0.154%, 0.153%, 0.1544% in sample to be tested；This implementation
The standard value of the mass content of phosphorus is 0.154% in standard sample to be measured used in example, tolerance 0.010%, the present invention
Offer detection molybdenum compound in phosphorus mass content method it is accurate to the testing result of phosphorus content, repeatability and repdocutbility compared with
It is good.
Embodiment 5 detects phosphorus content in GSB03-1689-2004 standard molybdenum-iron
3 detections are carried out according to method described in embodiment 1, testing result is that phosphorus mass content is distinguished in sample to be tested
It is 0.0360%, 0.0361%, 0.0345%；The standard of the mass content of phosphorus in standard sample to be measured used in the present embodiment
Value is 0.035%, tolerance 0.004%, and the method for phosphorus mass content contains phosphorus in detection molybdenum compound provided by the invention
The testing result of amount is accurate, and repeatability and repdocutbility are preferable.
Embodiment 6 detects phosphorus content in BH0314-4 (substitution) standard molybdenum-iron
Time detection is carried out according to method described in embodiment 1, testing result is that phosphorus mass content is in sample to be tested
0.0297%；The standard value of the mass content of phosphorus is 0.029% in standard sample to be measured used in the present embodiment, and tolerance is
0.0025%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is accurate to the testing result of phosphorus content.
Embodiment 7 detects phosphorus content in GSBC2013-57 standard molybdenum-iron
Time detection is carried out according to method described in embodiment 1, testing result is that phosphorus mass content is in sample to be tested
0.0359%；The standard value of the mass content of phosphorus is 0.036% in standard sample to be measured used in the present embodiment, and tolerance is
0.004%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is accurate to the testing result of phosphorus content.
Embodiment 8 detects phosphorus content in YSBC37653-10 standard molybdenum-iron
Time detection is carried out according to method described in embodiment 1, testing result is that phosphorus mass content is in sample to be tested
0.0458%；The standard value of the mass content of phosphorus is 0.046% in standard sample to be measured used in the present embodiment, and tolerance is
0.004%, the method provided by the invention for detecting phosphorus mass content in molybdenum compound is accurate to the testing result of phosphorus content.
Comparative example 1 detects phosphorus content in YSBC18605-08 standard molybdenum-iron
It is detected according to method as described in example 4, the difference with embodiment 4 is, the method for sample dissolution is：
Sample is placed in 300mL triangular flask or optical port beaker, 15 milliliters of nitric acid are added, after vigorous reaction, slowly by
Hydrofluoric acid is added dropwise in drop, and is heated to sample and is completely dissolved, and removes, and 3mL perchloric acid, 10mL sulfuric acid is added, continues to be heated to emitting sulphur
Sour 3~5min of white cigarette, is removed, cooling.35mL hydrochloric acid is added and dissolves by heating salt, moves into 500mL beaker, is diluted to warm water
250mL boils, and removes, slightly cold, has been neutralized to precipitating with ammonium hydroxide and has generated and cross plus 10mL, and low temperature boils 1min, remove standing to
Precipitating is sunk, and with the filtering of moderate qualitative filter paper, washs beaker, precipitating each 3~4 times with warm water.It is molten in several times with the hot sulfuric acid of 65mL
Solution is deposited in former beaker, and the precipitating on filter paper is cleaned with hot sulfuric acid lotion.Filtrate is moved into 100mL volumetric flask, is cooled to
Room temperature is diluted with water to scale, mixes.
Testing result is that phosphorus mass content is respectively 0.148%, 0.150%, 0.158% in sample to be tested；This comparative example
The standard value of the mass content of phosphorus is 0.154% in used standard sample to be measured, tolerance 0.010%.Comparative example mentions
The method of phosphorus mass content is relatively poor to the testing result of phosphorus content in the detection molybdenum compound of confession, repeatability and repdocutbility
Also poor, and detection process is complex, and the reagent of consumption is more, generates toxic perchloric acid cigarette.
As seen from the above embodiment, the present invention provides a kind of methods of phosphorus content in measurement molybdenum compound, including：It decomposes
Molybdenum compound sample, obtains decomposed solution；The reagent of the decomposition includes water, perchloric acid and hydrogen peroxide；By the decomposed solution into
Row colour developing, obtains developing solution；The developing solution is tested in the absorbance of 680~700nm wave-length coverage.Compared with prior art,
For measuring method provided by the invention during decomposition samples, the phosphorus in sample is directly pentavalent phosphorus by hydrogen peroxide oxidation,
Then phosphorus content is measured by blue spectrophotometry, it is easy to operate, and do not used during whole operation poisonous substance and
Toxic gas is generated, it is very environmentally friendly, and the interference of silicon is not present, test result is accurate.Measurement molybdenum chemical combination provided by the invention
The method of phosphorus content is easy to operate, quick, environmentally friendly in object, and testing result is accurate, is particularly suitable in detection molybdenum-iron or metal molybdenum
Phosphorus content.
What has been described above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of method of phosphorus content in measurement molybdenum compound, including：
Molybdenum compound sample is decomposed, decomposed solution is obtained；The reagent of the decomposition includes water, perchloric acid and hydrogen peroxide；
The decomposed solution is developed the color, developing solution is obtained；
The developing solution is tested in the absorbance of 680~700nm wavelength.
2. the method according to claim 1, wherein the molybdenum compound includes molybdenum-iron or metal molybdenum.
3. the method according to claim 1, wherein in the molybdenum compound phosphorus mass content be 0.01~
0.5%.
4. the method according to claim 1, wherein the hydrogen peroxide is hydrogenperoxide steam generator；The peroxide
The mass concentration for changing hydrogen solution is 25~35%.
5. the method according to claim 1, wherein the volume ratio of the water, perchloric acid and hydrogen peroxide is 40：
(15~25):(15~25).
6. the method according to claim 1, wherein the usage ratio of the molybdenum compound sample and reagent is
(0.2~0.3) g：(70~90) mL.
7. the method according to claim 1, wherein the method for the colour developing is：
The decomposed solution, hypo solution and mixed liquor are mixed, developing solution is obtained；
The mixed liquor includes：Perchloric acid, gum arabic solution, bismuth salt solution, ammonium molybdate solution and ascorbic acid solution.
8. the method according to the description of claim 7 is characterized in that the perchloric acid, bismuth salt solution, gum arabic solution,
The volume ratio of ammonium molybdate solution and ascorbic acid solution is 100:(25~45):(95~105):(95~105):(55~65).
9. the method according to the description of claim 7 is characterized in that the preparation method of the bismuth salt solution is：
Bismuth nitrate and perchloric acid are mixed, bismuth salt solution is obtained.
10. the method according to the description of claim 7 is characterized in that the concentration of the gum arabic solution is 15~25g/
L；
The concentration of the ammonium molybdate solution is 45~55g/L；
The concentration of the ascorbic acid solution is 95~105g/L；
The concentration of the hypo solution is 8~12g/L.
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