CN106596522A - Determination method for contents of silicon, manganese and phosphorus in natural microalloy iron powder - Google Patents
Determination method for contents of silicon, manganese and phosphorus in natural microalloy iron powder Download PDFInfo
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- CN106596522A CN106596522A CN201710113865.2A CN201710113865A CN106596522A CN 106596522 A CN106596522 A CN 106596522A CN 201710113865 A CN201710113865 A CN 201710113865A CN 106596522 A CN106596522 A CN 106596522A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention discloses a determination method for the contents of silicon, manganese and phosphorus in natural microalloy iron powder. The method comprises the following steps: 1) adding 50 to 80 ml of hydrochloric acid into per g of a to-be-determined sample of natural microalloy iron powder and carrying out low-temperature heating until the sample is dissolved so as to obtain a solution, wherein the hydrochloric acid has a volume ratio of HCl to H2O of 1: 2; 2) adding 200 mL of distilled water into per g of the solution obtained in the step (1) for volume fixation so as to obtain a sample solution containing silicon, manganese and phosphorus; and 3) carrying out determination, i.e., selecting the analysis spectral lines of silicon, manganese and phosphorus, determining the spectral line intensities of silicon, manganese and phosphorus in the sample solution by using an inductively coupled plasma-atomic emission spectrometer, and acquiring the corresponding content values of silicon, manganese and phosphorus from the standard work curves of silicon, manganese and phosphorus according to the spectral line intensities.
Description
Technical field
The invention belongs to analysis and testing technology field, and in particular to silicon in a kind of natural micro alloy iron powder, manganese, phosphorus content
Assay method.
Background technology
Natural micro alloy iron powder is a kind of brand-new powder metallurgy iron powder, and it has a series of other iron powder institutes incomparable
Advantage：Due to using unique vanadium titano-magnetite as raw material, the natural solid solution of iron powder have micro silicon, manganese, vanadium, titanium, nickel,
Cobalt, chromium, the alloying element of copper, create natural micro alloy iron powder product with the mechanicalness more remarkable than other iron powder products
Energy：Because using unique catalysis reduction grinding technique, granule-morphology is in the irregular of uniqueness under the mirror of natural micro alloy iron powder
Pod-like so that iron powder has thundering forming property, it is adaptable to which some have the application neck of particular/special requirement to forming property
Domain, while this also causes the granularmetric composition of iron powder to be more prone to control, can easily provide the natural micro alloy of different grain size composition
Iron powder, can be widely used in the fields such as powder metallurgy, medicine, environmental protection and chemical industry.
Silicon, manganese, the measure of phosphorus content in natural micro alloy iron powder, there is presently no the analysis method of standard.Element silicon
Analytic routines have gravimetric method, photometry etc., the analytic routines of manganese element has volumetric method, photometry, titration etc., a phosphorus unit
The analytic routines of element has gravimetric method, volumetric method, photometry, extraction spectrophotometric method etc..There is complex operation step in these methods, institute
Need chemical reagent more, some will also use organic reagent, impact operating personnel's is healthy, spent acid, salkali waste pollution environment,
The deficiencies such as analytical cycle length, and be difficult to meet production needs.ICP-AES be in recent years compared with
For ripe analysis method, with detection limit it is low, the degree of accuracy is good, matrix effect is little the features such as, can be used for the measure of low content.Adopt
Directly determined with ICP-AES silicon in natural micro alloy iron powder, manganese, phosphorus content difficulty compared with
Greatly, there is presently no effective method.
The content of the invention
It is an object of the invention to provide silicon, manganese, the assay method of phosphorus content in a kind of natural micro alloy iron powder.
The object of the present invention is achieved like this, comprises the following steps：
1）In natural micro alloy iron powder sample to be tested, hydrochloric acid is added, addition is the amount by 50～80mL/g samples, and low temperature adds
Heat to dissolving obtains solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
Beneficial effects of the present invention：
1st, the present invention solves the problems such as determining silicon, manganese, the larger phosphorus content difficulty in natural micro alloy iron powder, there is provided a kind of
With high accuracy, analyze speed is fast, and reagent dosage is few, and silicon, manganese in the little natural micro alloy iron powder of environmental pollution, phosphorus contain
The assay method of amount；The assay method that the present invention is adopted is simply effective, and amount of reagent is little, it is only necessary to a kind of reagent of hydrochloric acid, you can
Meet silicon, manganese, the measure needs of phosphorus content in daily natural micro alloy iron powder.
2nd, the method that the present invention is adopted is made after sample to be tested solution, you can use inductively coupled plasma of the prior art
Body Atomic Emission Spectrometer AES, is directly measured to the silicon in natural micro alloy iron powder, manganese, phosphorus content, and easy to operate, significantly
Detection cycle is shortened, detection efficiency is improve, the labour intensity of testing staff is alleviated, without the need for using a large amount of chemistry
Reagent, and avoid using concentrated hydrochloric acid and red fuming nitric acid (RFNA), actual bodily harm of the chemical reagent to testing crew is greatly reduced, also reduce
Chemical reagent pollution on the environment reduces cost.
3rd, silicon, manganese, the phosphorus content in natural micro alloy iron powder is determined using the present invention, its measurement result has good stablizing
Property, reappearance and accuracy.
Specific embodiment
With reference to embodiment, the present invention is further illustrated, but the present invention is any limitation as never in any form,
Based on present invention teach that any conversion for being made or replacement, belong to protection scope of the present invention.
Silicon, manganese, the assay method of phosphorus content, comprise the following steps in natural micro alloy iron powder of the present invention：
1）In natural micro alloy iron powder sample to be tested, hydrochloric acid is added, addition is the amount by 50～80mL/g samples, and low temperature adds
Heat to dissolving obtains solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
Step（1）Described in hydrochloric acid be analytically pure hydrochloric acid.
Step（1）Described in addition be amount by 60～70mL/g samples.
Step（1）Described in addition be amount by 65mL/g samples.
Step（3）Described in the condition of work of inductively coupled plasma atomic emission spectrometer be：Radio-frequency generator
RF power 1150W；Auxiliary gas flow amount 0.5L/min；Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed
50r/min；Integral number of times 3 times；Low band sweep time 15s；High band sweep time 8s.
Step（3）Described in selection silicon, manganese, phosphorus（Nm/ levels time）Analysis spectral line be silicon 251.611nm/134,
212.412nm/458；Manganese 257.610nm/131,259.373nm/130；Phosphorus 213.618nm/458,178.284nm/489.
Step（3）Described in the plot step of standard working curve of silicon be：
1）The preparation of standard liquid：Silica by purity more than 99.9% calcination 1h at 1000 DEG C, in being placed in drier
It is cooled to room temperature；By the amount of 5g/g samples, treated 2.1392g silica is placed in fill 7g it is finely ground and mix it is mixed
In closing the platinum crucible of flux, then mixed flux that is finely ground into 3g and mixing is covered, by platinum crucible prior to 400 DEG C of low-temperature heats, then at
950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux compares natrium carbonicum calcinatum for quality：Boric acid=2：1 mixed flux；So
During platinum crucible to be put into afterwards the beaker for filling 100mL cold water, frit is leached to after being completely dissolved, take out crucible, hot-cold lysis liquid
To room temperature；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to, is shaken up, moved in plastic bottle and protect
Deposit, obtain the silicon standard reserving solution of 1.00 mg/mL；Then silicon standard reserving solution is pipetted in 25mL to 100mL volumetric flasks, uses water
100mL is diluted to, is shaken up, obtain the silicon standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, silicon standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of silicon is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of silicon in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with silicon standard liquid, is painted
The standard working curve of silicon processed.
Step（3）Described in the plot step of standard working curve of manganese be：
1）The preparation of standard liquid：By the electrolytic manganese of purity more than 99.95%, it is put in sulfuric acid and cleans, treats that surface oxidation manganese is cleaned
Afterwards, take out, cleaned with distilled water, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is body
Product compares H2SO4：H2O=5:95；Above-mentioned treated 1.0000g electrolytic manganeses are placed in 250mL beakers, are tried by 30mL/g
The amount of sample, adds nitric acid, heating for dissolving to boil drive nitrogen oxides to the greatest extent in beaker, and hot-cold lysis liquid to room temperature, wherein nitric acid are
Volume ratio HNO3：H2O=1：1 nitric acid；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to,
Shake up, obtain the manganese containing solution of 1.00mg/mL；Manganese containing solution is pipetted in 25mL to 100mL volumetric flasks, is diluted with water to
100mL, shakes up, and obtains the manganese standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, manganese standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of manganese is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of manganese in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with manganese standard liquid, is painted
The standard working curve of manganese processed.
Step（3）Described in the plot step of standard working curve of phosphorus be：
1）The preparation of standard liquid：The pure potassium dihydrogen phosphate of commercially available benchmark is dried into 1h in 105～110 DEG C, is placed in cold in drier
But to room temperature；Above-mentioned treated 4.3936g potassium dihydrogen phosphates are placed in 500mL beakers；By 10mL/g potassium dihydrogen phosphates
Amount, then distilled water is added in beaker, boil, dissolving is complete, obtains lysate；Lysate is moved into into 1000mL volumetric flasks
In, 1000mL is diluted with water to, shake up, obtain the solution containing phosphate of 1.00mg/mL；Solution containing phosphate is pipetted into 25mL to 1000mL capacity
In bottle, 1000mL is diluted with water to, is shaken up, obtain the phosphorus standard liquid of 25.00ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, phosphorus standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of phosphorus is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of phosphorus in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with phosphorus standard liquid, is painted
The standard working curve of phosphorus processed.
Embodiment 1
Draw silicon, manganese, phosphorus standard working curve：
The plot step of the standard working curve of silicon is：
1）The preparation of standard liquid：Silica by purity more than 99.9% calcination 1h at 1000 DEG C, in being placed in drier
It is cooled to room temperature；By the amount of 5g/g samples, treated 2.1392g silica is placed in fill 7g it is finely ground and mix it is mixed
In closing the platinum crucible of flux, then mixed flux that is finely ground into 3g and mixing is covered, by platinum crucible prior to 400 DEG C of low-temperature heats, then at
950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux compares natrium carbonicum calcinatum for quality：Boric acid=2：1 mixed flux；So
During platinum crucible to be put into afterwards the beaker for filling 100mL cold water, frit is leached to after being completely dissolved, take out crucible, hot-cold lysis liquid
To room temperature；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to, is shaken up, moved in plastic bottle and protect
Deposit, obtain the silicon standard reserving solution of 1.00 mg/mL；Then silicon standard reserving solution is pipetted in 25mL to 100mL volumetric flasks, uses water
100mL is diluted to, is shaken up, obtain the silicon standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, silicon standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of silicon is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of silicon in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with silicon standard liquid, is painted
The standard working curve of silicon processed.
The plot step of the standard working curve of manganese is：
1）The preparation of standard liquid：By the electrolytic manganese of purity more than 99.95%, it is put in sulfuric acid and cleans, treats that surface oxidation manganese is cleaned
Afterwards, take out, cleaned with distilled water, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is body
Product compares H2SO4：H2O=5：95；Above-mentioned treated 1.0000g electrolytic manganeses are placed in 250mL beakers, are tried by 30mL/g
The amount of sample, adds nitric acid, heating for dissolving to boil drive nitrogen oxides to the greatest extent in beaker, and hot-cold lysis liquid to room temperature, wherein nitric acid are
Volume ratio HNO3：H2O=1：1 nitric acid；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to,
Shake up, obtain the manganese containing solution of 1.00mg/mL；Manganese containing solution is pipetted in 25mL to 100mL volumetric flasks, is diluted with water to
100mL, shakes up, and obtains the manganese standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, manganese standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of manganese is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of manganese in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with manganese standard liquid, is painted
The standard working curve of manganese processed.
The plot step of the standard working curve of phosphorus is：
1）The preparation of standard liquid：The pure potassium dihydrogen phosphate of commercially available benchmark is dried into 1h in 105 DEG C, is placed in drier and is cooled to room
Temperature；Above-mentioned treated 4.3936g potassium dihydrogen phosphates are placed in 500mL beakers；By the amount of 10mL/g potassium dihydrogen phosphates, then
Distilled water is added in beaker, is boiled, dissolving is complete, obtains lysate；Lysate is moved in 1000mL volumetric flasks, it is dilute with water
Release to 1000mL, shake up, obtain the solution containing phosphate of 1.00mg/mL；Solution containing phosphate is pipetted in 25mL to 1000mL volumetric flasks, water is used
1000mL is diluted to, is shaken up, obtain the phosphorus standard liquid of 25.00ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, phosphorus standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of phosphorus is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of phosphorus in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with phosphorus standard liquid, is painted
The standard working curve of phosphorus processed.
The measure of silicon, manganese, phosphorus content in natural micro alloy iron powder：
1）In natural micro alloy iron powder sample to be tested, hydrochloric acid is added, addition is the amount by 50mL/g samples, and low-temperature heat is extremely
Dissolving obtains solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid, described hydrochloric acid is analytically pure hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
The condition of work of the inductively coupled plasma atomic emission spectrometer described in the present embodiment is：Radio-frequency generator
RF power 1150W；Auxiliary gas flow amount 0.5L/min；Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed
50r/min；Integral number of times 3 times；Low band sweep time 15s；High band sweep time 8s.Described selection silicon, manganese, phosphorus（nm/
Level time）Analysis spectral line be silicon 251.611nm/134,212.412nm/458；Manganese 257.610nm/131,259.373nm/130；
Phosphorus 213.618nm/458,178.284nm/489.
Embodiment 2
Draw silicon, manganese, phosphorus standard working curve：
The plot step of the standard working curve of silicon is：
1）The preparation of standard liquid：Silica by purity more than 99.9% calcination 1h at 1000 DEG C, in being placed in drier
It is cooled to room temperature；By the amount of 5g/g samples, treated 2.1392g silica is placed in fill 7g it is finely ground and mix it is mixed
In closing the platinum crucible of flux, then mixed flux that is finely ground into 3g and mixing is covered, by platinum crucible prior to 400 DEG C of low-temperature heats, then at
950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux compares natrium carbonicum calcinatum for quality：Boric acid=2：1 mixed flux；So
During platinum crucible to be put into afterwards the beaker for filling 100mL cold water, frit is leached to after being completely dissolved, take out crucible, hot-cold lysis liquid
To room temperature；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to, is shaken up, moved in plastic bottle and protect
Deposit, obtain the silicon standard reserving solution of 1.00 mg/mL；Then silicon standard reserving solution is pipetted in 25mL to 100mL volumetric flasks, uses water
100mL is diluted to, is shaken up, obtain the silicon standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, silicon standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of silicon is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of silicon in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with silicon standard liquid, is painted
The standard working curve of silicon processed.
The plot step of the standard working curve of manganese is：
1）The preparation of standard liquid：By the electrolytic manganese of purity more than 99.95%, it is put in sulfuric acid and cleans, treats that surface oxidation manganese is cleaned
Afterwards, take out, cleaned with distilled water, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is body
Product compares H2SO4：H2O=5：95；Above-mentioned treated 1.0000g electrolytic manganeses are placed in 250mL beakers, are tried by 30mL/g
The amount of sample, adds nitric acid, heating for dissolving to boil drive nitrogen oxides to the greatest extent in beaker, and hot-cold lysis liquid to room temperature, wherein nitric acid are
Volume ratio HNO3：H2O=1：1 nitric acid；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to,
Shake up, obtain the manganese containing solution of 1.00mg/mL；Manganese containing solution is pipetted in 25mL to 100mL volumetric flasks, is diluted with water to
100mL, shakes up, and obtains the manganese standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, manganese standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of manganese is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of manganese in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with manganese standard liquid, is painted
The standard working curve of manganese processed.
The plot step of the standard working curve of phosphorus is：
1）The preparation of standard liquid：The pure potassium dihydrogen phosphate of commercially available benchmark is dried into 1h in 110 DEG C, is placed in drier and is cooled to room
Temperature；Above-mentioned treated 4.3936g potassium dihydrogen phosphates are placed in 500mL beakers；By the amount of 10mL/g potassium dihydrogen phosphates, then
Distilled water is added in beaker, is boiled, dissolving is complete, obtains lysate；Lysate is moved in 1000mL volumetric flasks, it is dilute with water
Release to 1000mL, shake up, obtain the solution containing phosphate of 1.00mg/mL；Solution containing phosphate is pipetted in 25mL to 1000mL volumetric flasks, water is used
1000mL is diluted to, is shaken up, obtain the phosphorus standard liquid of 25.00ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, phosphorus standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of phosphorus is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of phosphorus in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with phosphorus standard liquid, is painted
The standard working curve of phosphorus processed.
The measure of silicon, manganese, phosphorus content in natural micro alloy iron powder：
1）In natural micro alloy iron powder sample to be tested, hydrochloric acid is added, addition is the amount by 80mL/g samples, and low-temperature heat is extremely
Dissolving obtains solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid, described hydrochloric acid is analytically pure hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
The condition of work of the inductively coupled plasma atomic emission spectrometer described in the present embodiment is：Radio-frequency generator
RF power 1150W；Auxiliary gas flow amount 0.5L/min；Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed
50r/min；Integral number of times 3 times；Low band sweep time 15s；High band sweep time 8s.Described selection silicon, manganese, phosphorus（nm/
Level time）Analysis spectral line be silicon 251.611nm/134,212.412nm/458；Manganese 257.610nm/131,259.373nm/130；
Phosphorus 213.618nm/458,178.284nm/489.
Embodiment 3
Draw silicon, manganese, phosphorus standard working curve：
The plot step of the standard working curve of silicon is：
1）The preparation of standard liquid：Silica by purity more than 99.9% calcination 1h at 1000 DEG C, in being placed in drier
It is cooled to room temperature；By the amount of 5g/g samples, treated 2.1392g silica is placed in fill 7g it is finely ground and mix it is mixed
In closing the platinum crucible of flux, then mixed flux that is finely ground into 3g and mixing is covered, by platinum crucible prior to 400 DEG C of low-temperature heats, then at
950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux compares natrium carbonicum calcinatum for quality：Boric acid=2：1 mixed flux；So
During platinum crucible to be put into afterwards the beaker for filling 100mL cold water, frit is leached to after being completely dissolved, take out crucible, hot-cold lysis liquid
To room temperature；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to, is shaken up, moved in plastic bottle and protect
Deposit, obtain the silicon standard reserving solution of 1.00 mg/mL；Then silicon standard reserving solution is pipetted in 25mL to 100mL volumetric flasks, uses water
100mL is diluted to, is shaken up, obtain the silicon standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, silicon standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of silicon is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of silicon in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with silicon standard liquid, is painted
The standard working curve of silicon processed.
The plot step of the standard working curve of manganese is：
1）The preparation of standard liquid：By the electrolytic manganese of purity more than 99.95%, it is put in sulfuric acid and cleans, treats that surface oxidation manganese is cleaned
Afterwards, take out, cleaned with distilled water, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is body
Product compares H2SO4：H2O=5：95；Above-mentioned treated 1.0000g electrolytic manganeses are placed in 250mL beakers, are tried by 30mL/g
The amount of sample, adds nitric acid, heating for dissolving to boil drive nitrogen oxides to the greatest extent in beaker, and hot-cold lysis liquid to room temperature, wherein nitric acid are
Volume ratio HNO3：H2O=1：1 nitric acid；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to,
Shake up, obtain the manganese containing solution of 1.00mg/mL；Manganese containing solution is pipetted in 25mL to 100mL volumetric flasks, is diluted with water to
100mL, shakes up, and obtains the manganese standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, manganese standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of manganese is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of manganese in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with manganese standard liquid, is painted
The standard working curve of manganese processed.
The plot step of the standard working curve of phosphorus is：
1）The preparation of standard liquid：The pure potassium dihydrogen phosphate of commercially available benchmark is dried into 1h in 108 DEG C, is placed in drier and is cooled to room
Temperature；Above-mentioned treated 4.3936g potassium dihydrogen phosphates are placed in 500mL beakers；By the amount of 10mL/g potassium dihydrogen phosphates, then
Distilled water is added in beaker, is boiled, dissolving is complete, obtains lysate；Lysate is moved in 1000mL volumetric flasks, it is dilute with water
Release to 1000mL, shake up, obtain the solution containing phosphate of 1.00mg/mL；Solution containing phosphate is pipetted in 25mL to 1000mL volumetric flasks, water is used
1000mL is diluted to, is shaken up, obtain the phosphorus standard liquid of 25.00ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, phosphorus standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of phosphorus is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of phosphorus in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with phosphorus standard liquid, is painted
The standard working curve of phosphorus processed.
The measure of silicon, manganese, phosphorus content in natural micro alloy iron powder：
1）In natural micro alloy iron powder sample to be tested, hydrochloric acid is added, addition is the amount by 60mL/g samples, and low-temperature heat is extremely
Dissolving obtains solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid, described hydrochloric acid is analytically pure hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
The condition of work of the inductively coupled plasma atomic emission spectrometer described in the present embodiment is：Radio-frequency generator
RF power 1150W；Auxiliary gas flow amount 0.5L/min；Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed
50r/min；Integral number of times 3 times；Low band sweep time 15s；High band sweep time 8s.Described selection silicon, manganese, phosphorus（nm/
Level time）Analysis spectral line be silicon 251.611nm/134,212.412nm/458；Manganese 257.610nm/131,259.373nm/130；
Phosphorus 213.618nm/458,178.284nm/489.
Embodiment 4
Prepare following each standard liquid：
1st, the preparation of silicon standard liquid：
1A, the silica by purity more than the 99.9% calcination 1h at 1000 DEG C, is placed in drier and is cooled to room temperature；
1B, by the amount of 5g/g samples, the 2.1392g silica of step 1A is placed in the Carbon Dioxide for filling that 7g is finely ground and mixes
In the platinum crucible of the mixed flux of sodium and boric acid, then the natrium carbonicum calcinatum of and mixing finely ground into 3g and the mixed flux of boric acid are covered,
By crucible prior to 400 DEG C of low-temperature heats, then at 950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux are following mass ratio
Natrium carbonicum calcinatum：Boric acid=2：1；
1C, the platinum crucible in step 1B is put in the beaker for filling 100mL cold water, to leach frit to after being completely dissolved, is taken
Go out crucible, hot-cold lysis liquid is to room temperature；
1D, the lysate of step 1C is moved in 1000mL volumetric flasks, be diluted with water to 1000mL, shaken up, in moving into plastic bottle
Preserve, obtain the silicon standard reserving solution of 1.00 mg/mL；
1E, the solution in step 1D is pipetted in 25mL to 100mL volumetric flasks, be diluted with water to 100mL, shaken up, obtain 250ug/
The silicon standard liquid of mL.
2nd, the preparation of manganese standard liquid：
2A, by the electrolytic manganese of purity more than 99.95%, be put in sulfuric acid clean, after surface oxidation manganese clean after, take out, use distilled water
Clean, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is following volume ratio：H2SO4：
H2O=5：95；
2B, the 1.0000g electrolytic manganeses of step 2A are placed in 250mL beakers；
2C, by the amount of 30mL/g samples, add nitric acid in the beaker of step 2B, heating for dissolving boils drive nitrogen oxides to the greatest extent, cold
But to room temperature, wherein nitric acid is following volume ratio：HNO3 ：H2O=1：1；
2D, by step 2C solution move into 1000mL volumetric flasks in, be diluted with water to 1000mL, shake up, obtain 1.00mg/mL
Manganese containing solution；
2E, the solution in step 2D is pipetted in 25mL to 100mL volumetric flasks, be diluted with water to 100mL, shaken up, obtain 250ug/
The manganese standard liquid of mL.
3rd, the preparation of phosphorus standard liquid：
3A, by the pure potassium dihydrogen phosphate of commercially available benchmark in 106 DEG C dry 1h, be placed in drier and be cooled to room temperature；
3B, the 4.3936g potassium dihydrogen phosphates of step 3A are placed in 500mL beakers；
3C, by the amount of 10mL/g potassium dihydrogen phosphates, add distilled water in the beaker of step 3B, boil, dissolving is complete；
3D, by step 3C solution move into 1000mL volumetric flasks in, be diluted with water to 1000mL, shake up, obtain 1.00mg/mL's
Solution containing phosphate；
3E, the solution in step 3D is pipetted in 25mL to 1000mL volumetric flasks, be diluted with water to 1000mL, shaken up, obtained
25.00ug/mL phosphorus standard liquid.
4th, the preparation of solution is calibrated：
4A, weigh 5 parts of 0.5000g high purity irons and be respectively placed in 5 100mL volumetric flasks；
4B, in 5 volumetric flasks of 4A, add 30 mL hydrochloric acid, low-temperature heat to obtain solution to dissolving, wherein hydrochloric acid is following body
Product compares HCl: H2O=1:2；
4C, in the solution of step 4B, add the standard liquid of tested element by table 1, be diluted with water to scale, after mixing respectively
Obtain blank, mark 1, mark 2, mark 3,4 five calibration solution of mark.
The addition of the various elements of table 1
5th, the measure of inductively coupled plasma atomic emission spectrometer：
5A, instrumentation condition is optimized as follows：Radio-frequency generator RF power 1150W；Auxiliary gas flow amount 0.5L/min；
Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed 50r/min；Integral number of times 3 times；Low band sweep time
15s；High band sweep time 8s；Silicon, manganese, phosphorus（Nm/ levels time）Analysis spectral line be：Silicon 251.611nm/134,212.412nm/
458.Manganese 257.610nm/131,259.373nm/130.Phosphorus 213.618nm/458,178.284nm/489；
5B, respectively determination step 4C gained are blank, the intensity of spectral line of mark 1～4 standard liquids of mark；
, as abscissa, the intensity of spectral line is ordinate for 5C, concentration respectively with silicon, manganese, phosphorus titer in table 1, respectively draw silicon,
The working curve of manganese, phosphorus standard.
6th, silicon, manganese, the preparation of phosphorus test liquid in natural micro alloy iron powder to be measured：
6A, in 0.5000g natural micro alloy iron powder samples to be tested, by the amount of 60mL/g samples, add hydrochloric acid, low-temperature heat is extremely
Dissolving, obtains solution, and wherein hydrochloric acid is following volume ratio HCl：H2O=1：2；
6B, by the amount of 200mL/g samples, in the solution obtained by step 6A plus distilled water carry out constant volume to 100mL, that is, treated
Survey silicon, manganese, the test liquid of phosphorus content.
7th, silicon, manganese, the phosphorus yield in natural micro alloy iron powder to be measured：
7A, under with step 5A identical condition of work, the intensity of spectral line of determination step 6B gained sample liquids to be tested；
The intensity of spectral line of 7B, sample liquid to be tested according to measured by step 7A, find on the working curve of step 5C silicon, manganese,
Phosphorus content.
Claims (9)
1. silicon, manganese, the assay method of phosphorus content in a kind of natural micro alloy iron powder, it is characterised in that comprise the following steps：
1）In natural micro alloy iron powder sample to be tested, add hydrochloric acid, addition is the amount by 50～80mL/g samples, 40 DEG C with
Under be heated to dissolving and obtain solution, wherein hydrochloric acid is volume ratio HCl：H2O=1：2 hydrochloric acid；
2）By the amount of 200mL/g samples, in step（1）Gained solution in plus distilled water carry out constant volume, that is, obtain silicon to be measured,
The test liquid of manganese, phosphorus content；
3）Determine：Silicon, manganese, the analysis spectral line of phosphorus are selected, using inductively coupled plasma atomic emission spectrometer sample is determined
The intensity of spectral line of silicon, manganese, phosphorus in liquid, according to the intensity of spectral line obtain in silicon, manganese, the standard working curve of phosphorus corresponding silicon,
Manganese, phosphorus content value.
2. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（1）Described in hydrochloric acid be analytically pure hydrochloric acid.
3. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（1）Described in addition be amount by 60～70mL/g samples.
4. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（1）Described in addition be amount by 65mL/g samples.
5. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（3）Described in the condition of work of inductively coupled plasma atomic emission spectrometer be：Radio-frequency generator RF power
1150W；Auxiliary gas flow amount 0.5L/min；Vertical Observation height 12.0mm；Rinse pump speed 50r/min；Analysis pump speed 50r/
min；Integral number of times 3 times；Low band sweep time 15s；High band sweep time 8s.
6. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（3）Described in select silicon, manganese, phosphorus analysis spectral line be silicon 251.611nm/134,212.412nm/458；Manganese
257.610nm/131、259.373nm/130；Phosphorus 213.618nm/458,178.284nm/489.
7. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（3）Described in the plot step of standard working curve of silicon be：
1）The preparation of standard liquid：Silica by purity more than 99.9% calcination 1h at 1000 DEG C, in being placed in drier
It is cooled to room temperature；By the amount of 5g/g samples, treated 2.1392g silica is placed in fill 7g it is finely ground and mix it is mixed
In closing the platinum crucible of flux, then mixed flux that is finely ground into 3g and mixing is covered, by platinum crucible prior to 400 DEG C of low-temperature heats, then at
950 DEG C of high-temperature heating 40min, cooling, wherein mixed flux compares natrium carbonicum calcinatum for quality：Boric acid=2：1 mixed flux；So
During platinum crucible to be put into afterwards the beaker for filling 100mL cold water, frit is leached to after being completely dissolved, take out crucible, hot-cold lysis liquid
To room temperature；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to, is shaken up, moved in plastic bottle and protect
Deposit, obtain the silicon standard reserving solution of 1.00 mg/mL；Then silicon standard reserving solution is pipetted in 25mL to 100mL volumetric flasks, uses water
100mL is diluted to, is shaken up, obtain the silicon standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, silicon standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of silicon is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of silicon in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with silicon standard liquid, is painted
The standard working curve of silicon processed.
8. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（3）Described in the plot step of standard working curve of manganese be：
1）The preparation of standard liquid：By the electrolytic manganese of purity more than 99.95%, it is put in sulfuric acid and cleans, treats that surface oxidation manganese is cleaned
Afterwards, take out, cleaned with distilled water, place into and wash in absolute ethyl alcohol 4 times, taking-up is placed in drier and is dried, wherein sulfuric acid is body
Product compares H2SO4：H2O=5:95；Above-mentioned treated 1.0000g electrolytic manganeses are placed in 250mL beakers, are tried by 30mL/g
The amount of sample, adds nitric acid, heating for dissolving to boil drive nitrogen oxides to the greatest extent in beaker, and hot-cold lysis liquid to room temperature, wherein nitric acid are
Volume ratio HNO3：H2O=1：1 nitric acid；Above-mentioned lysate is moved in 1000mL volumetric flasks, 1000mL is diluted with water to,
Shake up, obtain the manganese containing solution of 1.00mg/mL；Manganese containing solution is pipetted in 25mL to 100mL volumetric flasks, is diluted with water to
100mL, shakes up, and obtains the manganese standard liquid of 250ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, manganese standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of manganese is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of manganese in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with manganese standard liquid, is painted
The standard working curve of manganese processed.
9. silicon, manganese, the assay method of phosphorus content in natural micro alloy iron powder according to claim 1, it is characterised in that step
Suddenly（3）Described in the plot step of standard working curve of phosphorus be：
1）The preparation of standard liquid：The pure potassium dihydrogen phosphate of commercially available benchmark is dried into 1h in 105～110 DEG C, is placed in cold in drier
But to room temperature；Above-mentioned treated 4.3936g potassium dihydrogen phosphates are placed in 500mL beakers；By 10mL/g potassium dihydrogen phosphates
Amount, then distilled water is added in beaker, boil, dissolving is complete, obtains lysate；Lysate is moved into into 1000mL volumetric flasks
In, 1000mL is diluted with water to, shake up, obtain the solution containing phosphate of 1.00mg/mL；Solution containing phosphate is pipetted into 25mL to 1000mL capacity
In bottle, 1000mL is diluted with water to, is shaken up, obtain the phosphorus standard liquid of 25.00ug/mL；
2）The preparation of calibration solution：Weigh 5 parts of 0.5000g high purity irons to be respectively placed in 5 100mL volumetric flasks；In 5 volumetric flasks
In, 30 mL hydrochloric acid are added, less than 40 DEG C are heated to dissolving, obtain solution, and wherein hydrochloric acid is volume ratio HCl：H2O=1：2；Then exist
In equipped with solution 5 volumetric flasks, phosphorus standard is added by 0.00 ml, 1.00 ml, 3.00 ml, 5.00 ml, 8.00 ml respectively
Solution, is diluted with water to scale, and 5 calibration solution are obtained final product after mixing；
3）The drafting of standard working curve：The analysis spectral line of phosphorus is selected, using inductively coupled plasma atomic emission spectrometer
The intensity of spectral line of phosphorus in 5 calibration solution is determined, as abscissa, the intensity of spectral line is ordinate to the concentration with phosphorus standard liquid, is painted
The standard working curve of phosphorus processed.
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