CN107271430A - A kind of method of inductively coupled plasma atomic emission spectrometry to aluminium, silicon, phosphorus simultaneous determination in ferro-boron - Google Patents
A kind of method of inductively coupled plasma atomic emission spectrometry to aluminium, silicon, phosphorus simultaneous determination in ferro-boron Download PDFInfo
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- CN107271430A CN107271430A CN201710605760.9A CN201710605760A CN107271430A CN 107271430 A CN107271430 A CN 107271430A CN 201710605760 A CN201710605760 A CN 201710605760A CN 107271430 A CN107271430 A CN 107271430A
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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 present invention relates to molding materials technical field of chemical detection, specifically related to a kind of inductively coupled plasma atomic emission spectrometry is to aluminium in ferro-boron, silicon, the method of phosphorus simultaneous determination, ferro-boron sample is with sodium carbonate, sodium peroxide, cleaned with water, plus hydrochloric acid acidifying, plus nitric acid dissolving, plus hydrogen-peroxide reduction, it is diluted to certain volume, then on inductively coupled plasma atomic emission (ICP AES) instrument, its emitted luminescence intensity is measured at the wavelength of recommended analytical line, the content of element to be measured is found by working curve, calculate the mass fraction of element to be measured.Silicon in ferro-boron, aluminium, the detection method of phosphorus are determined using ICP spectrographic techniques, its is simple to operate, take few, efficiency high, cost is low, and experimental precision is high.
Description
Technical field
The present invention relates to molding materials technical field of chemical detection, and in particular to a kind of inductively coupled plasma is former
Method of the sub- emission spectrometry to aluminium, silicon, phosphorus simultaneous determination in ferro-boron.
Background technology
Inductively coupled plasma atomic emission spectrometry is (referred to as：ICP spectroscopic methodologies) application field extensively, be commonly used to
In the sample analysis of water quality, environment, metallurgy, geology, chemicals, petrochemical industry, food and laboratory services etc..This method
Determine that elemental range is wide, H in the nonmetalloid such as C, N, O, F, Cl and alkali metal group that are excited except inert gas and some difficulties,
Outside Rb, Cs can not be detected, the element that can be analyzed has reached 78 kinds.
Aluminium, silicon, the phosphorus in ferro-boron are determined in existing method, is divided into three kinds of methods, respectively GB/T 3653.4-
2008EDTA volumetric methods survey aluminium, and GB/T 3653.6-1988 antimony P-Mo blue photometric method determines phosphorus amount and GB/T 3653.3-1988 are high
Chloric acid determination determines silicon amount.The above method is during composition measurement, and operating, time-consuming, to the behaviour of testing staff
Make technical requirements high, cost is high, detection error is big.
Therefore, based on above-mentioned, the present invention provide a kind of inductively coupled plasma atomic emission spectrometry to aluminium in ferro-boron,
The method of silicon, phosphorus simultaneous determination, silicon, aluminium, the detection efficiency of three kinds of elements of phosphorus and detection are improved by technical scheme
Precision, while sample preparation and sample detection operation difficulty are reduced, so as to solve the deficiency and defect of prior art presence.
The content of the invention
The purpose of the present invention is that：It is former there is provided a kind of inductively coupled plasma for the above mentioned problem that presently, there are
Sub- emission spectrometry improves silicon, aluminium, phosphorus three to the method for aluminium, silicon, phosphorus simultaneous determination in ferro-boron by technical scheme
The detection efficiency and accuracy of detection of element are planted, while sample preparation and sample detection operation difficulty are reduced, so as to solve existing skill
Deficiency and defect that art is present.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of inductively coupled plasma atomic emission spectrometry to the method for aluminium, silicon, phosphorus simultaneous determination in ferro-boron, including
Following steps：
(1) sample：0.1000 ± 0.0005g ferro-boron sample is weighed using precision weighing equipment, precision is weighed and is accurate to
0.0001g；
(2) sample melted：Ferro-boron sample is placed in nickel crucible, 0.6g natrium carbonicum calcinatums are added into crucible, and by nothing
Aqueous sodium carbonate is sufficiently mixed uniformly with ferro-boron sample, is subsequently placed in 600 DEG C of high temperature furnaces and is melted；After treating that sample is melted completely,
Sample is taken out and is cooled to room temperature, 0.9g sodium peroxides are added into sample, are placed in melting 10min in 800 DEG C of high temperature furnaces；Sample
After product melting completely, sample is taken out and shaken up, then 10min will be melted in sample 800 DEG C of high temperature furnaces of return, treat that sample melted is
During red, transparent melt state, sample is taken out, room temperature is cooled to；
(3) sample is acidified：The graduated transparent vessel of the tool of selection one, successively with acetone, absolute ethyl alcohol and deionized water
Clean up, the sample of cooling is transferred in transparent vessel, 10ml deionized waters are added into container, sample is cleaned, arrange
Go out deionized water；It is 1 according to volume ratio:1 hydrochloric acid mixed solution for preparing H2O and HCl is added in transparent vessel, and sample is acidified
Processing；It is 1 according to volume ratio after sample acidifying:1 prepares H2O and HNO3 nitric acid mixed solution, and transparent vessel is added
Heat, makes sample be dissolved in transparent vessel；When the liquid in transparent vessel becomes clarification, peroxidating is added dropwise into transparent vessel
Hydrogen, sample is reduced, and is subsequently cooled to room temperature；
(4) sample dilutes：It will reduce in the plastic containers that sample solution global transfer is 100ml to capacity, hold to plastics
Add deionized water to be diluted to 100ml in device, and dilute sample solution is shaken up, wait to be measured；
(5) prepared by standard liquid：Weigh 6 parts of high purity irons, the quality of every part of high purity iron is 0.0800g, and every part high-purity
Iron is respectively placed in nickel crucible, prepares standard liquid according to the method described in step (1) to step (5), and be contained in 100ml's
In plastic containers；6 parts of the standard liquid of silicon, aluminium, three kinds of materials of phosphorus is measured respectively, and the volume of 6 parts of standard liquids is respectively
0.00ml, 0.50ml, 1.00ml, 5.00ml, 10.00ml, 15.00ml, and every part of standard liquid constant volume in plastic containers adds
Water is to 100ml；
(6) composition measurement：Composition measurement is carried out to sample using ICP methods, in every part of standard liquid working curve
Each element analytical line emitted luminescence intensity is measured, respectively using the concentration of each analytical element as abscissa, and analysis line strength is vertical
Coordinate, drawing curve；Then spectroscopic assay is carried out to ferro-boron sample with ICP-AES instruments again, in recommended analytical line
Its emitted luminescence intensity is measured at wavelength, the content of element to be measured is found by working curve, the mass fraction of element to be measured is calculated.
Technical scheme, the preparation of sample and the preparation of standard liquid are on the one hand detected by ferro-boron, makes preparation
The sample detection degree of accuracy it is higher, for existing detection technique, sample preparation consumptive material of the invention is less, preparation side
Method operation is relatively simple, and preparation efficiency is higher, take it is less, beneficial to rapidly and efficiently preparing detection sample.
On the other hand, the present invention is melted by the way that ferro-boron sample is placed in nickel crucible, beneficial to by the part in sample
The volatile impurity of low melting point carries out melting volatilization, by way of melting and shaking up melt, can carry out sample mix
It is even, and realize that the diffusion of detection sample element is uniform by high temperature mode；And the hydrochloric acid acidifying and nitric acid by sample are dissolved, so
Afterwards by the reduction of hydrogen peroxide, the impurity in ferro-boron solution can be effectively removed, is more accurately detected beneficial to acquisition
As a result.
Another further aspect, the present invention is detected using ICP detection methods to sample composition, simple to operate, detection effect
Rate is high, and accuracy of detection is good；The silicon in ferro-boron is determined using ICP, the rate of recovery of phosphorus each element has reached standard GB/T/T
23942-2009《Chemical reagent inductively coupled plasma atomic emission spectrometry general rule》Element to be measured reclaims yield and should controlled
Scope requires that impurity element aluminium recovery also meets standard requirement of the control 50%~150% in 80%~120% standard；
Meanwhile, ICP spectroscopic methodologies working curve calibration, coefficient correlation is all higher than being equal to 0.99, it was demonstrated that detection method of the invention is reliable, accurate
Really, working curve is linearly good, can be for the silicon in measure ferro-boron, aluminium, phosphorus content；Technical scheme with it is existing
Manual humid analysis is compared, and its analysis efficiency can improve 60%, it is adaptable to detect the sample that silicon, aluminium content are less than 0.5%, and phosphorus contains
Sample of the amount more than 0.12%, detection method analysis result of the invention is accurate, with preferable application prospect.
It is preferred that, the precision weighing equipment in the step (1) is Precision Electronics Balance.
It is preferred that, the transparent vessel in the step (3) is specially the polytetrafluoroethylene beaker that capacity is 200ml.
It is preferred that, the plastic containers in the step (4) and step (5) are specially the plastics volumetric flask that capacity is 100ml.
It is preferred that, the hydrogen peroxide mass fraction in the step (3) is 30%, and the amount of the hydrogenperoxide steam generator of dropwise addition is
2-3 drops are added dropwise in standard dropper.It is preferred that,.
It is preferred that, the natrium carbonicum calcinatum in the step (2), the mass fraction of sodium carbonate is more than 99.8%, the peroxide
The mass fraction for changing sodium is more than 92.5%.
It is preferred that, in the high purity iron in the step (5), the mass fraction of ferro element is more than 99.9%.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：
Technical scheme, the preparation of sample and the preparation of standard liquid are on the one hand detected by ferro-boron, makes preparation
The sample detection degree of accuracy it is higher, for existing detection technique, sample preparation consumptive material of the invention is less, preparation side
Method operation is relatively simple, and preparation efficiency is higher, take it is less, beneficial to rapidly and efficiently preparing detection sample.
On the other hand, the present invention is melted by the way that ferro-boron sample is placed in nickel crucible, beneficial to by the part in sample
The volatile impurity of low melting point carries out melting volatilization, by way of melting and shaking up melt, can carry out sample mix
It is even, and realize that the diffusion of detection sample element is uniform by high temperature mode；And the hydrochloric acid acidifying and nitric acid by sample are dissolved, so
Afterwards by the reduction of hydrogen peroxide, the impurity in ferro-boron solution can be effectively removed, is more accurately detected beneficial to acquisition
As a result.
Another further aspect, the present invention is detected using ICP detection methods to sample composition, simple to operate, detection effect
Rate is high, and accuracy of detection is good；The silicon in ferro-boron is determined using ICP, the rate of recovery of phosphorus each element has reached standard GB/T/T
23942-2009《Chemical reagent inductively coupled plasma atomic emission spectrometry general rule》Element to be measured reclaims yield and should controlled
Scope requires that impurity element aluminium recovery also meets standard requirement of the control 50%~150% in 80%~120% standard；
Meanwhile, ICP spectroscopic methodologies working curve calibration, coefficient correlation is all higher than being equal to 0.99, it was demonstrated that detection method of the invention is reliable, accurate
Really, working curve is linearly good, can be for the silicon in measure ferro-boron, aluminium, phosphorus content；Technical scheme with it is existing
Manual humid analysis is compared, and its analysis efficiency can improve 60%, it is adaptable to detect the sample that silicon, aluminium content are less than 0.5%, and phosphorus contains
Sample of the amount more than 0.12%, detection method analysis result of the invention is accurate, with preferable application prospect.
Brief description of the drawings
Fig. 1 is testing process schematic diagram of the invention.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the present invention, rather than whole embodiments, based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Embodiment 1, as shown in Figure 1：
A kind of inductively coupled plasma atomic emission spectrometry to the method for aluminium, silicon, phosphorus simultaneous determination in ferro-boron, including
Following steps：
(1) sample：0.1000 ± 0.0005g ferro-boron sample is weighed using precision weighing equipment, precision is weighed and is accurate to
0.0001g；
(2) sample melted：Ferro-boron sample is placed in nickel crucible, 0.6g natrium carbonicum calcinatums are added into crucible, and by nothing
Aqueous sodium carbonate is sufficiently mixed uniformly with ferro-boron sample, is subsequently placed in 600 DEG C of high temperature furnaces and is melted；After treating that sample is melted completely,
Sample is taken out and is cooled to room temperature, 0.9g sodium peroxides are added into sample, are placed in melting 10min in 800 DEG C of high temperature furnaces；Sample
After product melting completely, sample is taken out and shaken up, then 10min will be melted in sample 800 DEG C of high temperature furnaces of return, treat that sample melted is
During red, transparent melt state, sample is taken out, room temperature is cooled to；
(3) sample is acidified：The graduated transparent vessel of the tool of selection one, successively with acetone, absolute ethyl alcohol and deionized water
Clean up, the sample of cooling is transferred in transparent vessel, 10ml deionized waters are added into container, sample is cleaned, arrange
Go out deionized water；It is 1 according to volume ratio:1 prepares H2O and HCl hydrochloric acid mixed solution is added in transparent vessel, and sample is acidified
Processing；It is 1 according to volume ratio after sample acidifying:1 prepares H2O and HNO3Nitric acid mixed solution, transparent vessel is heated,
Sample is set to be dissolved in transparent vessel；When the liquid in transparent vessel becomes clarification, hydrogen peroxide is added dropwise into transparent vessel,
Sample is reduced, room temperature is subsequently cooled to；
(4) sample dilutes：It will reduce in the plastic containers that sample solution global transfer is 100ml to capacity, hold to plastics
Add deionized water to be diluted to 100ml in device, and dilute sample solution is shaken up, wait to be measured；
(5) prepared by standard liquid：Weigh 6 parts of high purity irons, the quality of every part of high purity iron is 0.0800g, and every part high-purity
Iron is respectively placed in nickel crucible, prepares standard liquid according to the method described in step (1) to step (5), and be contained in 100ml's
In plastic containers；6 parts of the standard liquid of silicon, aluminium, three kinds of materials of phosphorus is measured respectively, and the volume of 6 parts of standard liquids is respectively
0.00ml, 0.50ml, 1.00ml, 5.00ml, 10.00ml, 15.00ml, and every part of standard liquid constant volume in plastic containers adds
Water is to 100ml；
(6) composition measurement：Composition measurement is carried out to sample using ICP methods, in every part of standard liquid working curve
Each element analytical line emitted luminescence intensity is measured, respectively using the concentration of each analytical element as abscissa, and analysis line strength is vertical
Coordinate, drawing curve；Then spectroscopic assay is carried out to ferro-boron sample with ICP-AES instruments again, in recommended analytical line
Its emitted luminescence intensity is measured at wavelength, the content of element to be measured is found by working curve, the mass fraction of element to be measured is calculated.
As the preferred scheme of the present embodiment, the precision weighing equipment in the step (1) is Precision Electronics Balance.
As the preferred scheme of the present embodiment, the transparent vessel in the step (3) is specially poly- four that capacity is 200ml
PVF beaker.
As the preferred scheme of the present embodiment, the plastic containers in the step (4) and step (5) are specially that capacity is
100ml plastics volumetric flask.
As the preferred scheme of the present embodiment, the hydrogen peroxide mass fraction in the step (3) is 30%, the mistake of dropwise addition
The amount of hydrogen peroxide solution is that 2 drops are added dropwise in standard dropper.It is preferred that,.
As the preferred scheme of the present embodiment, the natrium carbonicum calcinatum in the step (2), the mass fraction of sodium carbonate is more than
99.8%, the mass fraction of the sodium peroxide is more than 92.5%.
As the preferred scheme of the present embodiment, in the high purity iron in the step (5), the mass fraction of ferro element is more than
99.9%.
Calculated by the rate of recovery, silicon, the phosphorus in ferro-boron are determined using ICP, the rate of recovery of each element has reached national mark
Quasi- GB/T 23942-2009《Chemical reagent inductively coupled plasma atomic emission spectrometry general rule》Element to be measured reclaims yield
Control range is answered to be required in 80%~120% standard, as shown in table 1.
Silicon, aluminium, phosphorous recovery in the ferro-boron of table 1 are calculated
As seen from the table, the silicon in ferro-boron, the rate of recovery of phosphorus each element are determined using ICP and has reached standard GB/T/T
23942-2009《Chemical reagent inductively coupled plasma atomic emission spectrometry general rule》Element to be measured reclaims yield and should controlled
Scope requires that impurity element aluminium recovery also meets standard requirement of the control 50%~150% in 80%~120% standard.
Specific embodiment 2, as shown in Figure 1：
A kind of inductively coupled plasma atomic emission spectrometry to the method for aluminium, silicon, phosphorus simultaneous determination in ferro-boron, including
Following steps：
(1) sample：0.1000 ± 0.0005g ferro-boron sample is weighed using precision weighing equipment, precision is weighed and is accurate to
0.0001g；
(2) sample melted：Ferro-boron sample is placed in nickel crucible, 0.6g natrium carbonicum calcinatums are added into crucible, and by nothing
Aqueous sodium carbonate is sufficiently mixed uniformly with ferro-boron sample, is subsequently placed in 600 DEG C of high temperature furnaces and is melted；After treating that sample is melted completely,
Sample is taken out and is cooled to room temperature, 0.9g sodium peroxides are added into sample, are placed in melting 10min in 800 DEG C of high temperature furnaces；Sample
After product melting completely, sample is taken out and shaken up, then 10min will be melted in sample 800 DEG C of high temperature furnaces of return, treat that sample melted is
During red, transparent melt state, sample is taken out, room temperature is cooled to；
(3) sample is acidified：The graduated transparent vessel of the tool of selection one, successively with acetone, absolute ethyl alcohol and deionized water
Clean up, the sample of cooling is transferred in transparent vessel, 10ml deionized waters are added into container, sample is cleaned, arrange
Go out deionized water；It is 1 according to volume ratio:1 prepares H2O and HCl hydrochloric acid mixed solution is added in transparent vessel, and sample is acidified
Processing；It is 1 according to volume ratio after sample acidifying:1 prepares H2O and HNO3Nitric acid mixed solution, transparent vessel is heated,
Sample is set to be dissolved in transparent vessel；When the liquid in transparent vessel becomes clarification, hydrogen peroxide is added dropwise into transparent vessel,
Sample is reduced, room temperature is subsequently cooled to；
(4) sample dilutes：It will reduce in the plastic containers that sample solution global transfer is 100ml to capacity, hold to plastics
Add deionized water to be diluted to 100ml in device, and dilute sample solution is shaken up, wait to be measured；
(5) prepared by standard liquid：Weigh 6 parts of high purity irons, the quality of every part of high purity iron is 0.0800g, and every part high-purity
Iron is respectively placed in nickel crucible, prepares standard liquid according to the method described in step (1) to step (5), and be contained in 100ml's
In plastic containers；6 parts of the standard liquid of silicon, aluminium, three kinds of materials of phosphorus is measured respectively, and the volume of 6 parts of standard liquids is respectively
0.00ml, 0.50ml, 1.00ml, 5.00ml, 10.00ml, 15.00ml, and every part of standard liquid constant volume in plastic containers adds
Water is to 100ml；
(6) composition measurement：Composition measurement is carried out to sample using ICP methods, in every part of standard liquid working curve
Each element analytical line emitted luminescence intensity is measured, respectively using the concentration of each analytical element as abscissa, and analysis line strength is vertical
Coordinate, drawing curve；Then spectroscopic assay is carried out to ferro-boron sample with ICP-AES instruments again, in recommended analytical line
Its emitted luminescence intensity is measured at wavelength, the content of element to be measured is found by working curve, the mass fraction of element to be measured is calculated.
As the preferred scheme of the present embodiment, the precision weighing equipment in the step (1) is Precision Electronics Balance.
As the preferred scheme of the present embodiment, the transparent vessel in the step (3) is specially poly- four that capacity is 200ml
PVF beaker.
As the preferred scheme of the present embodiment, the plastic containers in the step (4) and step (5) are specially that capacity is
100ml plastics volumetric flask.
As the preferred scheme of the present embodiment, the hydrogen peroxide mass fraction in the step (3) is 30%, the mistake of dropwise addition
The amount of hydrogen peroxide solution is that 3 drops are added dropwise in standard dropper.It is preferred that,.
As the preferred scheme of the present embodiment, the natrium carbonicum calcinatum in the step (2), the mass fraction of sodium carbonate is more than
99.8%, the mass fraction of the sodium peroxide is more than 92.5%.
As the preferred scheme of the present embodiment, in the high purity iron in the step (5), the mass fraction of ferro element is more than
99.9%.
Calibration curve is operated using above-mentioned ICP spectroscopic methodologies, coefficient correlation is all higher than 0.99, is shown in Table 2.Prove this method
Reliably, accurately, working curve is linearly good, can be for the silicon in measure ferro-boron, aluminium, phosphorus.Compared with manual humid analysis
Efficiency can improve 60%, it is adaptable to detect the sample that silicon, aluminium content are less than 0.5%, and phosphorus content is more than 0.12% sample, method
Analysis result is accurate.
| Element | Wavelength | Intercept | Slope | Curvature | Coefficient correlation |
| Si | 251.611 | 87466.0 | 200700 | 0.00000 | 0.997211 |
| Al | 396.153 | 446735.3 | 724500 | 0.00000 | 0.997460 |
| P | 177.434 | 516.5 | 1886 | 0.00000 | 0.997190 |
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art can readily occur in change or replacement in the technical scope of present disclosure, should all contain
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (7)
1. a kind of inductively coupled plasma atomic emission spectrometry is to the method for aluminium, silicon, phosphorus simultaneous determination in ferro-boron, its feature
It is：Comprise the following steps：
(1) sample：0.1000 ± 0.0005g ferro-boron sample is weighed using precision weighing equipment, precision is weighed and is accurate to
0.0001g；
(2) sample melted：Ferro-boron sample is placed in nickel crucible, 0.6g natrium carbonicum calcinatums are added into crucible, and by anhydrous carbon
Sour sodium is sufficiently mixed uniformly with ferro-boron sample, is subsequently placed in 600 DEG C of high temperature furnaces and is melted；After treating that sample is melted completely, by sample
Product are taken out and are cooled to room temperature, and 0.9g sodium peroxides are added into sample, are placed in melting 10min in 800 DEG C of high temperature furnaces；Sample is complete
After full-fusing, sample is taken out and shaken up, then 10min will be melted in sample 800 DEG C of high temperature furnaces of return, it is red to treat sample melted
During clear melt state, sample is taken out, room temperature is cooled to；
(3) sample is acidified：The graduated transparent vessel of the tool of selection one, is cleaned with acetone, absolute ethyl alcohol and deionized water successively
Totally, the sample of cooling is transferred in transparent vessel, 10ml deionized waters is added into container, sample is cleaned, discharged
Ionized water；It is 1 according to volume ratio:1 prepares H2O and HCl hydrochloric acid mixed solution is added in transparent vessel, at sample acidifying
Reason；It is 1 according to volume ratio after sample acidifying:1 prepares H2O and HNO3Nitric acid mixed solution, transparent vessel is heated, made
Sample is dissolved in transparent vessel；When the liquid in transparent vessel becomes clarification, hydrogen peroxide is added dropwise into transparent vessel, will
Sample is reduced, and is subsequently cooled to room temperature；
(4) sample dilutes：It will reduce in the plastic containers that sample solution global transfer is 100ml to capacity, into plastic containers
Plus deionized water is diluted to 100ml, and dilute sample solution is shaken up, wait to be measured；
(5) prepared by standard liquid：Weigh 6 parts of high purity irons, the quality of every part of high purity iron is 0.0800g, and every part of high purity iron point
It is not placed in nickel crucible, prepares standard liquid according to the method described in step (1) to step (5), and be contained in 100ml plastics
In container；Measure 6 parts of the standard liquid of silicon, aluminium, three kinds of materials of phosphorus respectively, the volumes of 6 parts of standard liquids be respectively 0.00ml,
0.50ml, 1.00ml, 5.00ml, 10.00ml, 15.00ml, and every part of standard liquid constant volume in plastic containers adds water to
100ml；
(6) composition measurement：Composition measurement is carried out to sample using ICP methods, to each member in every part of standard liquid working curve
Plain analytical line emitted luminescence intensity is measured, respectively using the concentration of each analytical element as abscissa, and analysis line strength is ordinate,
Drawing curve；Then spectroscopic assay is carried out to ferro-boron sample with ICP-AES instruments again, at the wavelength of recommended analytical line
Its emitted luminescence intensity is measured, the content of element to be measured is found by working curve, the mass fraction of element to be measured is calculated.
2. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：Precision weighing equipment in the step (1) is Precision Electronics Balance.
3. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：Transparent vessel in the step (3) is specially that the polytetrafluoroethylene (PTFE) that capacity is 200ml burns
Cup.
4. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：Plastic containers in the step (4) and step (5) are specially the plastics that capacity is 100ml
Volumetric flask.
5. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：Hydrogen peroxide mass fraction in the step (3) is 30%, and the hydrogen peroxide of dropwise addition is molten
The amount of liquid is that 2-3 drops are added dropwise in standard dropper.
6. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：Natrium carbonicum calcinatum in the step (2), the mass fraction of sodium carbonate is more than 99.8%, institute
The mass fraction for stating sodium peroxide is more than 92.5%.
7. a kind of inductively coupled plasma atomic emission spectrometry as claimed in claim 1 is combined to aluminium, silicon, phosphorus in ferro-boron
Method for measuring, it is characterised in that：In high purity iron in the step (5), the mass fraction of ferro element is more than 99.9%.
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| CN109738419A (en) * | 2018-12-18 | 2019-05-10 | 郑州磨料磨具磨削研究所有限公司 | The measuring method of boron content in a kind of aluminum-based boron carbide material |
| CN110687060A (en) * | 2019-10-24 | 2020-01-14 | 攀钢集团江油长城特殊钢有限公司 | Method for combined determination of phosphorus and silicon content in high-carbon ferrochrome and nitrided ferrochrome |
| CN112630210A (en) * | 2020-11-02 | 2021-04-09 | 阳春新钢铁有限责任公司 | Method for jointly measuring silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma |
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| CN112630210A (en) * | 2020-11-02 | 2021-04-09 | 阳春新钢铁有限责任公司 | Method for jointly measuring silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma |
| CN112683621A (en) * | 2020-12-28 | 2021-04-20 | 唐山钢铁集团有限责任公司 | Method for detecting content of silicon element in manganese-silicon alloy |
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