CN106290318A - ICP AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously - Google Patents
ICP AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously Download PDFInfo
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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
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N21/714—Sample nebulisers for flame burners or plasma burners
Abstract
The present invention relates to analysis and testing technology field, particularly measure the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore with inductively coupled plasma emission spectrography (ICP AES) simultaneously, specifically lithium metaborate is a kind of high-melting-point non-oxidisable solvents, most of samples there is the strongest capacity of decomposition, it is possible to effectively decompose rock and the mineral of some indissolubles.The present invention is that phosphorus ore sample is in platinum crucible, add lithium metaborate solvent and lithium bromide releasing agent high frequency molten model machine fusion and decomposition phosphorus ore sample, during under magnetic stirring apparatus, high temperature pours the polytetrafluoroethylene beaker filling 10% nitric acid into, after the most molten sample acidifying constant volume, country-level phosphorus ore standard substance is used to carry out Matrix Match and Y Int Std method Criterion curve, ICP AES measures phosphorus pentoxide in phosphorus ore simultaneously, magnesium oxide, ferrum oxide, aluminium oxide, silicon dioxide, calcium oxide, titanium dioxide, manganese oxide, the method of strontium oxide content, it is convenient to have, the advantage such as accurately, it is particularly suited for batch phosphorus ore sample determination.
Description
Technical field
The present invention relates to a kind of ICP-AES method and measure the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously, belong to
Analysis and testing technology field.
Background technology
In rock phosphate in powder, multielement analyzes the chemical method that general employing is traditional, i.e. GB/T1870～1881-1995 phosphorus ore
Stone and the sampling of phosphorus concentrate can only detect single-element with sample preparation and chemical analysis method, operate tediously long.Sample pre-treatments, one
As be divided into that alkali is molten and acid is molten, produce a large amount of waste liquid simultaneously, can not meet high-volume and quickly analyze requirement.
ICP-AES spectrum analysis is molten to phosphorus, magnesium, ferrum, aluminum, silicon, calcium, titanium, manganese, the requirement of strontium pre-treatment in phosphorus ore sample
Solving completely, without solid residue and suspended substance, decomposition method dissolves method, and mineral acid, Fluohydric acid. and mineral acid nitration mixture decompose
Method two class.Fusion method introduces a large amount of salts, it is necessary to dilution for many times method reduces solution salinity, causes extension rate the highest, shadow
Ring detection limit and the mensuration of Minor element.Mineral acid cannot aluminum, silicon in decomposing phosphate rock sample, Fluohydric acid. and mineral acid mix completely
Acid decomposition is due to silicon volatilization loss in sample, and can not measure the content of silicon.
In rock phosphate in powder, phosphorus, magnesium, ferrum, aluminum, silicon, calcium, titanium, manganese, strontium single element standard solution and sample solution are at matrix element
Composition, the aspect such as total salinity be difficult to keep consistent, cause both viscosity, proportion and surface tension variant.Due to solution
The factor such as viscosity, proportion and surface tension ICP-AES is measured during atomization process, mist droplet particle size, aerocolloidal biography
Defeated and solvent evaporation has an impact, if standard solution and sample to be tested solution are in the composition of matrix element, total salinity, acidity
Etc. aspect there are differences, the significant change of the intensity of spectral line will be caused during mensuration, cause measurement error bigger.
Summary of the invention
The invention aims to overcome the defect of prior art, it is provided that a kind of method is easy, quick, the ICP-of environmental protection
AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously.
ICP-AES method of the present invention measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously, is logical
Cross what below scheme realized:
The most accurately weigh 0.1000g phosphorus ore sample to be put in platinum crucible, by phosphorus ore: the ratio of lithium metaborate=1:10-20
Example, adds lithium metaborate mixing to phosphorus ore sample, adds 10 lithium-bromide solutions, be placed on the molten model machine of high frequency, pre-at 700 DEG C
Oxidation 2min, makes reduzate fully oxidized, and then liter high-temperature is to 1050 DEG C, after dissolving 2min, takes out platinum earthenware with Crucible tongs
Crucible, directly pours in the 400mL polytetrafluoroethylene beaker filling 100mL salpeter solution by fervid molten pearl, polytetrafluoroethyl-ne immediately
Alkene beaker on magnetic stirring apparatus by burst for tiny particle dissolution completely after, cooling, hold in 250mL with deionized water constant volume
In measuring bottle, measure for ICP-AES；
The most accurately weigh 0.1000g country-level phosphorus ore standard substance to be put in platinum crucible, add 1.2g lithium metaborate
Mixing, adds 10 lithium-bromide solutions, is placed on the molten model machine of high frequency, pre-oxidizes 2min at 700 DEG C, makes reduzate fully oxidized,
Then liter high-temperature is to 1050 DEG C, after dissolving 2min, takes out platinum crucible with Crucible tongs, is directly poured into by fervid molten pearl immediately
Fill in the 400mL polytetrafluoroethylene beaker of 100mL salpeter solution, polytetrafluoroethylene beaker will burst on magnetic stirring apparatus into
After tiny particle dissolution is complete, cooling, with deionized water constant volume in 250mL volumetric flask, do blank assay in company with sample, obtain
Obtain standard solution, measure for ICP-AES；
C. the country-level phosphorus ore standard substance standard solution prepared in step b is used hydrofluoric acid resistant on ICP-AES
Nebulizer sample introduction, carries software with instrument and carries out Matrix Match, spectral line interference and Y Int Std method Criterion curve, finally use
Inductively coupled plasma emission spectrography measures.
Lithium metaborate described in step a is GR level；Lithium bromide is GR level, and mass concentration is 400g/L；Nitric acid is GR level, body
Fraction is 10%；Magnetic stirring apparatus rotates to be 450 turns/min.
Country-level phosphorus ore standard substance described in described step b be GBW07210, GBW07211, GBW07212,
The mass ratio of GBW07210+GBW07212 is that 1:1 mixture standard substance forms standard series.
Use Y Int Std method Criterion curve described in described step c, yttrium standard solution is GR level, and mass concentration is 10 μ
g/mL。
Above-mentioned steps instrument equipment: direct-reading plasma emission spectrometer composed entirely by iCAP7400 type；Hydrofluoric acid resistant mist
Change device；The molten model machine of Analymate-V4D high frequency.
Inductively coupled plasma emission spectrography is that the class atom with induction coupled plasma torch as excitation source is sent out
Penetrate spectroscopic analysis methods, be a kind of novel analytical technology being derived by atomic emission spectrometry.Can easily and fast, accurate
Really carrying out multielement analysis simultaneously, measure sensitivity higher, detection limit is relatively low, has good precision and repeatability, is
Measure the suitable apparatus of phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore sample.
Through test of many times, when processing phosphorus ore sample, use lithium metaborate solvent, add lithium bromide releasing agent 1050
Dissolve after the acidifying of 4min nitric acid extracts constant volume on DEG C molten model machine of high frequency, utilize Matrix Match and eliminate dry from modes such as peak buckle back scapes
Disturb, choose hydrofluoric acid resistant nebulizer sample introduction directly with five oxidation two in inductance coupled plasma optical emission spectrographic determination phosphorus ore
Phosphorus, magnesium oxide, ferric oxide, alchlor, silicon dioxide, calcium oxide, potassium oxide, sodium oxide, titanium dioxide, manganese oxide, oxygen
Change content of strontium.
In the inventive method selects, solvent and sample and thinner ratio, releasing agent selection, molten sample temperature, solution acidity are carried out
With condition tests such as stabilities of solution, the analysis conditions such as incident wavelength, atomizing pressure, incident power, lifting capacity are carried out excellent
Choosing.This method detection is limited to 0.0002～0.024 μ g/g, and relative standard deviation is 0.48%～1.32%, and the present invention has anti-
The features such as interference performance is strong, range of linearity width, precision are high, result is accurate, it is adaptable to rock phosphate in powder phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese strontium
The quick analysis of content.
Beneficial effects of the present invention is as follows:
Use lithium metaborate to make solvent, the molten model machine of high frequency dissolves, the method for high temperature acidified test solution in advance.Use inductance coupling
Close plasma emission spectrometry (ICP-AES) and quickly measure containing of the elements such as phosphorus, magnesium, ferrum, aluminum, silicon, calcium, titanium, manganese, strontium in phosphorus ore
Amount, have between matrix effect element to be measured little, each do not substantially interfere with, sample pre-treatments simple to operate, solve tradition molten
The problem that silicone content can not be measured by quadrat method simultaneously, this law greatly increases work efficiency simultaneously, reduces energy consumption, has
Good application prospect and bigger economic benefit.
Detailed description of the invention
ICP-AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously, device therefor instrument:
Direct-reading plasma emission spectrometer composed entirely by iCAP7400 type；Hydrofluoric acid resistant nebulizer；The molten model machine of Analymate-V4D high frequency,
Specifically comprise the following steps that
The most accurately weigh 0.1000g phosphorus ore sample to be put in platinum crucible, add the mixing of 1.2g lithium metaborate, add 10
Lithium-bromide solution, is placed on the molten model machine of high frequency, pre-oxidizes 2min at 700 DEG C, makes reduzate fully oxidized, then rises high-temperature extremely
1050 DEG C, after dissolving 2min, take out platinum crucible with Crucible tongs, fervid molten pearl is directly poured into fill 100mL nitric acid immediately
In the 400mL polytetrafluoroethylene beaker of solution, polytetrafluoroethylene beaker is molten by bursting the microgranule for tiny on magnetic stirring apparatus
After solving completely, cooling, with deionized water constant volume in 250mL volumetric flask, measure for ICP-AES；
The most accurately weigh 0.1000g country-level phosphorus ore standard substance to be put in platinum crucible, add 1.2g lithium metaborate
Mixing, adds 10 lithium-bromide solutions, is placed on the molten model machine of high frequency, pre-oxidizes 2min at 700 DEG C, makes reduzate fully oxidized,
Then liter high-temperature is to 1050 DEG C, after dissolving 2min, takes out platinum crucible with Crucible tongs, is directly poured into by fervid molten pearl immediately
Fill in the 400mL polytetrafluoroethylene beaker of 100mL salpeter solution, polytetrafluoroethylene beaker will burst on magnetic stirring apparatus into
After tiny particle dissolution is complete, cooling, with deionized water constant volume in 250mL volumetric flask, do blank assay in company with sample, supply
ICP-AES measures；
C. the country-level phosphorus ore standard substance standard solution prepared in step b is used hydrofluoric acid resistant on ICP-AES
Nebulizer sample introduction, carries software with instrument and carries out Matrix Match, spectral line interference and Y Int Std method Criterion curve, finally use
Inductively coupled plasma emission spectrography measures.
In this rapid assay methods:
1. the preparation of standard solution series
Accurately weigh 0.1000g country-level phosphorus ore standard substance GBW07210 (standard 2), GBW07211 (standard 3),
GBW07212 (standard 4), the mass ratio of GBW07210+GBW07212 (standard 5) are that 1:1 mixture standard substance forms standard system
Row.It is put in platinum crucible, adds the mixing of 1.2g lithium metaborate, add 10 lithium-bromide solutions, be placed on the molten model machine of high frequency,
700 DEG C of pre-oxidation 2min, make reduzate fully oxidized, and then liter high-temperature is to 1050 DEG C, after dissolving 2min, takes out with Crucible tongs
Platinum crucible, directly pours in the 400mL polytetrafluoroethylene beaker filling 100mL salpeter solution by fervid molten pearl immediately, poly-
Tetrafluoroethene beaker on magnetic stirring apparatus by burst for tiny particle dissolution completely after, cooling, with deionized water constant volume in
In 250mL volumetric flask, doing blank assay (standard 1) in company with sample, preparing standard solution concentration is shown in Table 1.
Table 1 concentration of standard solution w/%
| Phosphorus ore component | Standard 1 | Standard 2 | Standard 3 | Standard 4 | Standard 5 |
| Phosphorus pentoxide (P2O5) | 0 | 36.89 | 20.86 | 6.06 | 21.48 |
| Magnesium oxide (MgO) | 0 | 0.43 | 8.19 | 7.12 | 3.78 |
| Iron sesquioxide (Fe2O3) | 0 | 1.04 | 1.08 | 3.08 | 2.06 |
| Aluminium sesquioxide (Al2O3) | 0 | 0.58 | 2.58 | 4.06 | 2.32 |
| Silicon dioxide (SiO2) | 0 | 3.26 | 3.61 | 38.8 | 21.03 |
| Calcium oxide (CaO) | 0 | 51.32 | 40.71 | 19.42 | 35.37 |
| Titanium dioxide (TiO2) | 0 | 0.037 | 0.14 | 0.48 | 0.26 |
| Manganese oxide (MnO) | 0 | 0.024 | 0.015 | 0.026 | 0.025 |
| Strontium oxide (SrO) | 0 | 0.077 | 0.16 | 0.055 | 0.066 |
2. solvent and the thinner ratio of sample
Test the solvent of 20:1,15:1,12:1,10:1,8:1 and 5:1 and the thinner ratio of sample respectively.Found that:
When thinner ratio is 5:1,8:1, sample not readily dissolves and the demoulding, and when thinner ratio is 10:1,12:1,15:1,20:1, sample is readily soluble
Solve and stripping result is preferable.Rock phosphate in powder is mainly phosphorus, silicon, magnesium, calcium, ferrum, aluminum as important master containing secondary element, is therefore judging
During experiment parameter quality, select phosphorus, silicon, magnesium, calcium, ferrum, aluminum as object of study, have chosen GBW07212 standard substance (w (P2O5)
=6.06%, w (SiO2)=38.80%, w (MgO)=7.12%, w (CaO)=19.42%, w (Fe2O3)=3.08%, w
(Al2O3)=4.06%) under the conditions of the different thinner ratio such as 10:1,12:1,15:1,20:1, dissolve preparation examination according to experimental technique
Liquid, measures P in phosphorus ore with ICP-AES2O5、SiO2、MgO、CaO、Fe2O3、Al2O3The situation of change of mass fraction, and as
According to selecting optimal proportion, it is shown in Table 2.
Main content element determination result w/% during the different thinner ratio of table 2
From table 2 result of the test: along with thinner ratio raises, P2O5、SiO2, CaO measurement result gradually rise, solvent with
The thinner ratio of sample measurement result in the range of 10:1～12:1 can be accepted.Therefore thinner ratio determines at 12:1, can save
Solvent load, it is possible to take into account the salinity impact on measurement result.
3. melt sample temperature
In the rock phosphate in powder that experiment relates to, phosphorus, magnesium, ferrum, aluminum, silicon, calcium, titanium, manganese, strontium are at high temperature respectively provided with the most stable
Property, under the conditions of the molten sample temperature of laboratory observation is respectively 850,950,1050,1150 DEG C, sample dissolves situation, when molten sample temperature sets
When being set to 850,950 DEG C, after the 2min melting time terminates, sample segment dissolves not exclusively, when temperature is set in 1050,1150
DEG C time, sample can be completely dissolved in melt stage, therefore melts sample temperature and is set as 1050 DEG C.
4. selection and the addition of releasing agent is tested
Halogen compounds is considered as most effective releasing agent, such as bromide LiBr, NH4Br etc. and iodide KI, NH4I etc..
It is found by experiment that LiBr stripping result and mobility are preferable.LiBr releasing agent, LiBr solution is selected by test further
(400g/L) easy demoulding when addition is 200mg (about 10), the molten pearl of noresidue in platinum crucible.To phosphorus in rock phosphate in powder, magnesium,
Ferrum, aluminum, silicon, calcium, titanium, manganese, strontium equal size measure noiseless.
5. the selection of solution acidity
Owing to the sample of inductance coupling plasma emissioning spectral analysis is solution, the therefore viscosity of solution, density and table
All evaporations to atomization process, droplet size and solvent such as surface tension have an impact；And along with the increase of acidity so that unit to be measured
Element emissive porwer reduces, therefore, as far as possible with low concentration acid.This experiment HNO to 2%, 5%, 10%, 15%3Contrasted
Experiment, finds the HNO of 10%3The ability of sample dissolution is preferable, and solution acidity finally uses the HNO of 4%3Medium.
6. solution stability testing
The apatite of China is mainly with fluor-apatite (3Ca3(PO4)2·CaF2) it is main.Due in solution matrix containing silicon,
Fluorine, potassium, sodium and other elements that can produce salt exist, in the preparation process of solution, it is possible to silicon, fluorine, potassium, sodium are situated between in acidity
Matter easily produces localized agglomeration presented in colloid.In order to beneficially sample extraction is complete, this experiment is taked to add 10mL
The sample after dissolving is extracted in nitric acid acidifying, tests the stability of silicon in solution.Under experimental conditions, if mistake standing time
Long (more than 24h), by the low side for the measurement result causing silicon.So should measure as early as possible after prepared by sample.
7. analysis spectral line
In rock phosphate in powder, macroelement is relatively big due to concentration difference, should be according to sample composition and constituent content, from instrument software
In the element spectral line to be measured that spectral line storehouse is recommended, several sensitive lines of element to be measured are selected to screen.Selection peak shape is good, interference
Simple, the highly sensitive spectral line of little, background the results are shown in Table 3 as analytical line, the final analysis spectral line selected.
The each element analysis spectrum line of table 3
| Element | Wavelength/nm | Background correction mode |
| P | 213.618 | Left |
| Ca | 317.933 | Right |
| Mg | 285.213 | Left and right |
| Si | 251.612 | Left and right |
| Fe | 259.940 | Left and right |
| Al | 396.152 | Left and right |
| Ti | 334.941 | Left and right |
| Mn | 257.610 | Left and right |
| Sr | 407.771 | Right |
8. instrument and running parameter
Direct-reading plasma emission spectrometer echelle grating composed entirely by iCAP7400 type；Two-dimensional array (CID) detector；High
Salt nebulizer.Instrument working parameter is: high-frequency emission power: 1150W；Cooling gas flow 12L/min；Secondary air amount 0.5L/
min；Nebulizer pressure 0.2MPa；Observed altitude 12mm；Rinse pump speed 50r/min；Wriggling pump speed 50r/min；Sample lifting capacity
1.5mL/min；Sample wash time 30s；The time of integration: shortwave 7s, long wave 5s.
9. calibration curve and detection limit
Standard solution series is measured by the working condition set according to instrument, with the mass concentration of element to be measured as horizontal stroke
Coordinate, emissive porwer is vertical coordinate, draws calibration curve.Linear equation and linearly dependent coefficient, be shown in Table 4.At the optimal bar of instrument
To blank solution METHOD FOR CONTINUOUS DETERMINATION 10 times under work package, with the detection limit of element to be measured each in 3 times of standard deviation calculation methods, result
It is shown in Table 4.
Table 4 linear equation, correlation coefficient and detection limit
10. precision and recovery test
According to P in determination of experimental method phosphorus ore sample CY-182O5、MgO、Fe2O3、Al2O3、SiO2、CaO、TiO2、MnO、
SrO constituent content, and carry out precision and mark-on recovery test, the results are shown in Table 5.As can be seen from Table 5: measurement result is marked relatively
Quasi-deviation (RSD, n=10) is between 0.48%～1.32%, and the response rate is 97%～102%, is satisfied by analyzing test request.
Table 5 precision and recovery test result
| Component | Measured value w/% | Relative standard deviation RSD (n=10)/% | Add scalar w/% | Measure total amount w/% | The response rate/% |
| P2O5 | 24.72 | 0.72 | 20.00 | 44.56 | 99 |
| CaO | 36.51 | 0.63 | 20.00 | 56.38 | 99 |
| MgO | 2.05 | 0.51 | 2.00 | 4.02 | 98 |
| SiO2 | 26.98 | 0.69 | 20.00 | 46.69 | 98 |
| Fe2O3 | 1.17 | 0.48 | 1.00 | 2.16 | 99 |
| Al2O3 | 0.64 | 0.82 | 1.00 | 1.62 | 98 |
| TiO2 | 0.032 | 1.32 | 0.030 | 0.061 | 97 |
| MnO | 0.042 | 1.16 | 0.040 | 0.083 | 102 |
| SrO | 0.066 | 1.04 | 0.060 | 0.127 | 102 |
11. sample analysis
Determining CY-14, tri-rock phosphate in powder samples of CY-15, CY-16 by ICP-AES method, table 6 result shows, measured value with
Chemical score is consistent, and shows that this method is highly sensitive, and precision is good with accuracy, it is adaptable to the analysis of rock phosphate in powder.
Table 6 rock phosphate in powder standard substance is analyzed.
Claims (4)
1.ICP-AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously, it is characterised in that its method
For:
The most accurately weigh 0.1000g phosphorus ore sample to be put in platinum crucible, in phosphorus ore: the ratio of lithium metaborate=1:10-20, to
Phosphorus ore sample adds lithium metaborate mixing, adds and reenters 10 lithium-bromide solutions, be placed on the molten model machine of high frequency, 700 DEG C of pre-oxidation
2min, makes reduzate fully oxidized, and then liter high-temperature is to 1050 DEG C, after melted 2min, takes out platinum crucible with Crucible tongs, vertical
Bead that will be fervid is directly poured in the 400mL polytetrafluoroethylene beaker filling 100mL salpeter solution, polytetrafluoroethylene beaker
On magnetic stirring apparatus by burst for tiny particle dissolution completely after, cooling, with deionized water constant volume in 250mL volumetric flask
In, measure for ICP-AES；
The most accurately weigh 0.1000g country-level phosphorus ore standard substance to be put in platinum crucible, add the mixing of 1.2g lithium metaborate,
Add 10 lithium-bromide solutions, be placed on the molten model machine of high frequency, pre-oxidize 2min at 700 DEG C, make reduzate fully oxidized, then rise
High-temperature, to 1050 DEG C, after dissolving 2min, takes out platinum crucible with Crucible tongs, is directly poured into by fervid molten pearl immediately and fills
In the 400mL polytetrafluoroethylene beaker of 100mL salpeter solution, polytetrafluoroethylene beaker will burst as tiny on magnetic stirring apparatus
Particle dissolution completely after, cooling, with deionized water constant volume in 250mL volumetric flask, do blank assay in company with sample, it is thus achieved that mark
Quasi-solution, measures for ICP-AES；
C. the country-level phosphorus ore standard substance standard solution prepared in step b is atomized with hydrofluoric acid resistant on ICP-AES
Device sample introduction, carries software with instrument and carries out Matrix Match, spectral line interference and Y Int Std method Criterion curve, finally use inductance
Coupled plasma optical emission spectrographic determination.
ICP-AES method the most according to claim 1 measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously,
It is characterized in that,
Step a weighs phosphorus ore 0.1000g,
Lithium metaborate described in step a is GR level；Lithium bromide is GR level, and mass concentration is 400g/L；Nitric acid is GR level, volume integral
Number is 10%；Magnetic stirring apparatus rotates to be 450 turns/min.
ICP-AES method the most according to claim 1 measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously,
It is characterized in that, the country-level phosphorus ore standard substance described in step b be GBW07210, GBW07211, GBW07212,
The mass ratio of GBW07210+GBW07212 is that 1:1 mixture standard substance forms standard series.
ICP-AES method the most according to claim 1 measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously,
It is characterized in that, the use Y Int Std method Criterion curve described in step c, yttrium standard solution is GR level, and mass concentration is 10 μ g/
mL。
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| CN110161015A (en) * | 2019-05-29 | 2019-08-23 | 云南磷化集团有限公司 | The method for measuring phosphorus magnesium-ferrum-aluminum calcium manganese titanium oxide content in black shale |
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| CN110161015A (en) * | 2019-05-29 | 2019-08-23 | 云南磷化集团有限公司 | The method for measuring phosphorus magnesium-ferrum-aluminum calcium manganese titanium oxide content in black shale |
| CN110161015B (en) * | 2019-05-29 | 2022-02-18 | 云南磷化集团有限公司 | Method for determining content of phosphorus-magnesium-iron-aluminum-calcium-manganese-titanium oxide in black shale |
| CN110779781A (en) * | 2019-11-12 | 2020-02-11 | 江苏宝众宝达药业有限公司 | Method for measuring total amount of magnetic foreign matters in battery-grade lithium hydroxide monohydrate by ICP method |
| CN111122549A (en) * | 2020-01-06 | 2020-05-08 | 包头钢铁（集团）有限责任公司 | Method for measuring magnesium oxide, potassium oxide, manganese oxide, titanium oxide and silicon dioxide in limestone and dolomite |
| CN111999281A (en) * | 2020-07-07 | 2020-11-27 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of silicon, manganese and titanium in ferrophosphorus by ICP-AES method |
| CN116718585A (en) * | 2023-05-05 | 2023-09-08 | 北京先通国际医药科技股份有限公司 | Method for determining oxide content in yttrium-containing glass microspheres and application of melting agent in determination of oxide content in yttrium-containing glass microspheres |
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