CN108872203A - The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag - Google Patents
The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag Download PDFInfo
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- CN108872203A CN108872203A CN201811146528.4A CN201811146528A CN108872203A CN 108872203 A CN108872203 A CN 108872203A CN 201811146528 A CN201811146528 A CN 201811146528A CN 108872203 A CN108872203 A CN 108872203A
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The detection method of elemental composition, belongs to Element detection analysis technical field in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag.A kind of digestion procedure of vanadium chromium slag is used for inductively coupled plasma atomic emission spectrometry detection elements ingredient, and vanadium chromium slag and basic solvent mixed melting are obtained fusant, and acid solution is added after fusant is cooling and dissolves by heating.Inductively coupled plasma atomic emission spectrometry detection elements ingredient is used for by the way that solution is made in the resolution of vanadium chromium slag.The slightly solubilities oxides such as titanium dioxide, aluminum oxide, silica and chrome green for indissoluble in vanadium chromium slag, the present invention, which is reacted under high-temperature fusion using vanadium chromium slag with basic solvent, generates salt, then the method dissolved with acid solution.Effectively slightly solubility oxide can be dissolved, the solid not dissolved is avoided to generate error to later period measurement element.Furthermore the invention further relates to a kind of a kind of detection methods of elemental composition in vanadium chromium slag sample and measurement vanadium chromium slag.
Description
Technical field
The present invention relates to Element detection analysis technical fields, and in particular to a kind of vanadium chromium slag and its digestion procedure and one kind
Measure the detection method of elemental composition in vanadium chromium slag.
Background technique
China is richly stored with v-ti magnetite ore resources, and only the domestic vanadium titano-magnetite proven reserve in Sichuan is just
It is the vanadium and titanium resources storage site of largest domestic up to 73.37 hundred million tons, while also gives birth to many high prices such as chromium cobalt nickel gallium niobium scandium with (same)
Beneficial element, resource preciousness must be comprehensively utilized substantially efficiently.The red mining area Ge Nan of Panxi Diqu belongs to chromium type high v-ti magnetite
Mine, wherein iron, vanadium grade are suitable with the grade in other mining areas, and the content of chromium is then 8~10 times of other mining areas, Hongge Deposit area
Become since the prior art is still not enough to sufficiently extract a variety of valuable metal elements simultaneously and climb the big v-ti magnetite mining area in Xisi (too
With mine, Bai Makuang, mining heritages, Hongge Deposit) among unique not yet large-scale development in the mining area utilized is temporarily limited, urgently
One of critical issue of solution is exactly efficient, economy, cleanly extraction and separation vanadium chromium resource from the mineral of natural endowment vanadium chromium.
Research direction is the process flow using " blast furnace ironmaking-vanadium extraction by converter blowing chromium " at present, and vanadium and chromium coexist in the process
In slag phase (vanadium chromium slag), it is the raw material of further recycling vanadium, chromium, researchs and solves and extract and separate to economical and efficient from vanadium chromium slag
Vanadium, chromium are then key problem in technology, and the exploitation that vanadium chromium extracts with isolation technics needs the support of correlation detection technology, to quick and precisely
Grasp the content and variation of elemental composition in vanadium chromium slag in ground.
The measurement of usual elemental composition is that suitable detection and analysis technology, general constant are selected according to the height of its content
Element is using instruments analysis sides such as traditional chemical analysis method or x ray fluorescence spectrometry (XRF) such as gravimetric method, titrations
Method, microelement using the traditional chemical analysis method or atomic absorption spectrography (AAS) (AAS), inductive coupling etc. such as spectrophotometry from
Daughter atom emission spectrometry (ICP-AES).
When being used to measure solution middle and high concentration elemental composition using ICP-AES, need that Specimen eliminating is first prepared into original
After beginning solution, then artificially ICP-AES is reduced to fit constituent content to be measured in original solution using dividing to take and dilute step by step again
The mode of suitable measurement range further prepares sample detection solution, finally by element in measurement sample detection solution content again
Be able to calculate the content of element to be measured in primary sample multiplied by extension rate, thus cause the precision of testing result be deteriorated and
Error is amplified with extension rate.Therefore, measuring elemental composition in vanadium chromium slag is also to select phase respectively according to the height of constituent content
Detection technique is answered, Main elements mostly use X ray fluorescence spectra (XRF) to survey sial vanadium titanium, or with traditional chemical analysis method weight
Amount method surveys silicon, ammonium ferric sulfate or ferrous ammonium sulfate titration and surveys vanadium-titanium-chromium, EDTA compleximetry survey aluminium.Usually mostly use ICP-
AES measures the micro constitutents such as the vanadium chromium in vanadium chromium slag sample less than 1.0%, and its sample solution resolution preparation method mostly uses
Hydrofluoric acid, chloroazotic acid (hydrochloric acid is added：Nitric acid=3：1), perchloric acid and water and the heating progress Specimen eliminating on electric hot tray, and hold
It is continuous to be heated at high temperature to perchloric acid decomposing solution and eliminate hydrofluoric acid in wet salt to drive, diluted hydrochloric acid dissolution salt is added, finally with
Water dilutes after constant volume with the content of ICP-AES measurement micro impurity element, not only Specimen eliminating preparation flow up to 4~5h but also
Not exclusively there is sour insoluble residue in Specimen eliminating, it is higher and with dioxy that content in sample can not be cleared up completely and be measured to such method
Change slightly solubility oxide component to be measured existing for the forms such as titanium, three three aluminium of oxidation, silica, chrome green.
Summary of the invention
The first object of the present invention is to provide a kind of digestion procedure of vanadium chromium slag, this digestion procedure is simple, and what is obtained disappears
Solution sample can be used in inductively coupled plasma atomic emission spectrometry detection elements ingredient.
The second object of the present invention is to provide a kind of vanadium chromium slag sample, for inductively coupled plasma body atomic emissions light
Spectrometry detection elements ingredient.
The third object of the present invention is to provide a kind of detection method of elemental composition in measurement vanadium chromium slag, can be directly same
When measurement vanadium chromium slag sample in content be 0.01~15.0% Si, Al, V, Ti, Cr and Na element content, it is very simple
Just.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of digestion procedure of vanadium chromium slag, detects for inductively coupled plasma atomic emission spectrometry
Elemental composition comprising：
Vanadium chromium slag and basic solvent mixed melting are obtained into fusant, it is molten that acid solution heating is added after fusant is cooling
Solution.
The present invention proposes a kind of vanadium chromium slag sample, clears up to obtain according to the digestion procedure of above-mentioned vanadium chromium slag.
The present invention proposes a kind of detection method for measuring elemental composition in vanadium chromium slag, using inductively coupled plasma body atom
Content is 0.01~15.0% Si, Al, V, Ti, Cr and Na in the above-mentioned vanadium chromium slag sample of transmitting spectrometry Simultaneous Direct Determination
The content of element.
The beneficial effect of the embodiment of the present invention is：
A kind of digestion procedure of vanadium chromium slag provided by the invention is used for inductive coupling by the way that solution is made in the resolution of vanadium chromium slag
Plasma atomic emission spectrometry detection elements ingredient.For titanium dioxide, aluminum oxide, the dioxy of indissoluble in vanadium chromium slag
The slightly solubilities oxide such as SiClx and chrome green, the present invention react generation with basic solvent using vanadium chromium slag under high-temperature fusion
Salt, then the method dissolved with acid solution.Effectively slightly solubility oxide can be dissolved, avoid the solid not dissolved
Error is generated to later period measurement element.
A kind of vanadium chromium slag sample provided by the invention can be used in inductively coupled plasma atomic emission spectrometry detection
Elemental composition.
The detection method of elemental composition in a kind of measurement vanadium chromium slag provided by the invention, being capable of Simultaneous Direct Determination vanadium chromium slag
Content is the content of 0.01~15.0% Si, Al, V, Ti, Cr and Na element in sample, avoids every kind of element and individually surveys
Fixed tedious steps, it is very easy.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to elemental composition in a kind of vanadium chromium slag of the embodiment of the present invention and its digestion procedure and a kind of measurement vanadium chromium slag
Detection method be specifically described.
The present invention provides a kind of digestion procedure of vanadium chromium slag, detects for inductively coupled plasma atomic emission spectrometry
Elemental composition comprising：
1, basic solvent is prepared
It is in powdered for taking natrium carbonicum calcinatum and boric acid to grind respectively, is 4 according to mass ratio：1 by natrium carbonicum calcinatum and boric acid
It is uniformly mixed and is placed in 110~120 DEG C of environment dry 1~2h.
It is 4 that basic solvent, which takes mass ratio,：1 natrium carbonicum calcinatum and mebor, can make titanium dioxide in vanadium chromium slag,
The slightly solubilities oxides such as three three aluminium of oxidation, silica, chrome green can quickly form salt in high-temperature fusion, be dissolved in acid
In property solution.Wherein sodium carbonate mainly plays flux effect, and boric acid plays fluxing agent effect.
Basic solvent be ground into it is uniform powdered, when basic solvent purity is inadequate, in subsequent detection elemental composition
It can also be by taking the influence deducted and contain element blank background to be measured in the simple measures such as reagent blank elimination basic solvent.
2, it pre-oxidizes
It is 1 according to mass ratio：5 heat vanadium chromium slag and basic solvent uniformly mixed be placed in container, are passed through air, add
Heat is to 300~400 DEG C of 10~15min of reaction.
Guarantee to keep aerobic environment in heating container by being passed through air, makes the metal simple-substance in vanadium chromium slag and aoxidize at a low price
Object is substantially oxidized to high oxide, its alloy is avoided to react or corrode valuable platinum crucible vessel.Furthermore it is possible to avoid
Some simple substance for being not dissolved in acid solution cannot be resolved the elemental composition influenced in subsequent measurements vanadium chromium slag completely, generate
Error.
Since basic solvent dosage is only 5 times that sample weighs quality, flux dosage is when far below usual frit reaction
Thus the relationship that 10~30 times of sample quality substantially reduces the introduced matrix effect of Specimen eliminating reagent, background interference, blank
The influence factors such as background, accuracy and the precision for improving ICP-AES measurement constituent content are horizontal.
3, frit reaction
Fusant is obtained after being continuously heating to 950~1000 DEG C of 20~25min of reaction.
Melting by the slightly solubilities oxides such as titanium dioxide in vanadium chromium slag, three three aluminium of oxidation, silica, chrome green with
Basic solvent forms the salt for being soluble in acid solution under high-temperature fusion.Rejecting slightly solubility oxide is avoided individually to carry out element survey
It is fixed, simplify detecting step.
4, it dissolves by heating
It is cooled to room temperature to fusant, acid solution is added, be uniformly mixed, be heated to 95~97 DEG C, it is complete to fusant
Stop heating after dissolution, obtains lysate；
Acid solution includes any one or two kinds in dilute hydrochloric acid and dust technology；
Dilute hydrochloric acid is that the concentrated hydrochloric acid that mass percent concentration is 36~38% is matched according to 1 part of concentrated hydrochloric acid and 2 parts of deionized waters
It is made；
Dust technology is that the concentrated nitric acid that mass percent concentration is 65~68% is matched according to 1 part of concentrated nitric acid and 2 parts of deionized waters
It is made；
250~300mL acid solution is added in every gram of vanadium chromium slag.
The condition of the acidity of the acid solution of addition, liquor capacity and heating temperature can ensure that fusant can be quickly complete
Fully dissolved, while also avoiding the components such as the silicate of solution middle and high concentration, titanate generation hydrolysis and being condensed into as indissoluble
Property the forms such as silica, titanium dioxide be precipitated, ensured the real reliability of testing result.Because generation silica,
After the Precipitations such as titanium dioxide, the measurement of Si, Ti element is not only directly seriously affected, but also its co-precipitation or absorption are mingled with
Effect will also influence the measurement result of other not facile hydrolysis elements.
5, constant volume
Liquid to be dissolved is cooled to room temperature, with deionized water dilution constant volume lysate, the deionized water of vanadium chromium slag and constant volume
Mass volume ratio is 0.3~0.5g/L.
Preferably due to the capacity of various laboratory apparatus limits, for example, constant volume volumetric flask capacity and in order to guarantee
Measure the accuracy of each element ingredient in vanadium chromium slag.In the resolution sample of a vanadium chromium slag, 0.10~0.20g of vanadium chromium slag is weighed
Pre-oxidation and frit reaction are carried out with 0.50g~1.00g basic solvent, 25~30mL acid leach solution is added.
Vanadium chromium slag takes the dosage for the various reagents being added in 0.10~0.20g and subsequent resolution reaction, will be in solution
The concentration of introduced alkali metal potassium ion etc. reduces regulation to reasonable level, simply in sample matrices component and basic solvent
Effectively eliminate the components such as alkali metal ion of easily ionizable excitation in sample matrices composition and basic solvent complicated and changeable
The interference effects factors such as caused matrix effect, continuous background superposition；And the ratio between sample quality and constant volume
Relationship not only ensures that concentration of the high-content matrix component in sample solution can be adjusted control and existed by disposable dilution operation
Optimal level within ICP-AES determination of the upper limit, while also taking into account to avoid and generating script content with regard to lower microelement quilt
Excess dilution and lower than ICP-AES Determination Limit and can not Accurate Determining the problem of, in conjunction be preferably suitable for sensitivity divide
It analyses the ICP-AES detection parameters such as spectral line, meets while measuring 0.01~15.0% matrix component and micronutrient levels
It needs, solves and solution is carried out to take diluted mode of operation to lead to testing result accuracy precision level variation etc. for multiple point step by step
Problem.
The present invention provides a kind of vanadium chromium slag sample, clears up to obtain according to the digestion procedure of above-mentioned vanadium chromium slag.
This vanadium chromium slag resolution sample meets while measuring 0.01~15.0% matrix component and micronutrient levels
It needs, can be used in inductively coupled plasma atomic emission spectrometry (ICP-AES) while measuring multiple element ingredient.
The present invention provides a kind of detection method for measuring elemental composition in vanadium chromium slag, using inductively coupled plasma body atom
Content is 0.01~15.0% Si, Al, V, Ti, Cr and Na element in transmitting spectrometry Simultaneous Direct Determination vanadium chromium slag sample
Content.
The calibration curve standard solution of method is more without the complexity of vanadium chromium slag, vanadium chromium slag according to contained in sample solution
Become matrix composition and basic solvent and its concentration carries out Matrix Match interference correction, is directly used with the standard solution of each element to be measured
Water dilution be configured to concentration be respectively 0.00%, 0.010%, 0.100%, 0.500%, 1.00%, 5.00%, 10.0%,
The serial mixed standard solution of 8 of 15.0% draws working curve calibration ICP-AES instrument with this.Also, it is preferred that element to be measured
Analysis spectral line Si 251.611nm, Al 396.152nm, V 310.230nm, Ti 337.280nm, Cr 205.560nm, Na
589.592nm。
ICP-AES detection parameters RF power 1100W, secondary air speed 1.0L/min, peristaltic pump pump speed 58r/min, observation
Height 11.6mm, nebulizer pressure 0.23MPa, 10~15s of the time of integration.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The embodiment of the present invention provides a kind of a kind of inspection of elemental composition in vanadium chromium slag and its digestion procedure and measurement vanadium chromium slag
Survey method.
1, basic solvent is prepared
It is in powdered for taking natrium carbonicum calcinatum and boric acid to grind respectively, is 4 according to mass ratio：1 by natrium carbonicum calcinatum and boric acid
It is uniformly mixed and is placed in 120 DEG C of environment dry 2h.
2, it pre-oxidizes
Take respectively 0.10g vanadium chromium slag and 0.50g basic solvent be placed in platinum crucible be uniformly mixed be placed in Muffle furnace,
It is passed through air, is heated to 350 DEG C of reaction 12min.
3, frit reaction
Fusant is obtained after being continuously heating to 980 DEG C of reaction 20min.
4, it dissolves by heating
It is cooled to room temperature to fusant, 25mL hydrochloric acid solution is added, be uniformly mixed, be placed in electric hot plate low-temperature heat to 95 DEG C
State close to boiling stops heating after fusant is completely dissolved, obtains lysate.
5, constant volume
Liquid to be dissolved is cooled to room temperature, and is diluted to volume in 250mL volumetric flask with deionized water and is uniformly mixed, vanadium chromium slag is made
Sample.
6, each element content in vanadium chromium slag is measured
Measure the content of the elements such as Si, Al, V, Ti, Cr, Na in vanadium chromium slag sample solution simultaneously using ICP-AES.Using
Directly the standard solution of each element to be measured is diluted with water be configured to concentration be 0.00%, 0.010%, 0.100%, 0.500%,
1.00%, the serial mixed standard solution of 8 of 5.00%, 10.0%, 15.0% is molten as no Matrix Match calibration curve standard
Liquid calibrates ICP-AES spectrometer with this and draws working curve.ICP-AES detection parameters, which are arranged, is：Analysis spectral line Si
251.611nm, Al 396.152nm, V 310.230nm, Ti 337.280nm, Cr 205.560nm, Na 589.592nm, RF
Power 1100W, secondary air speed 1.0L/min, peristaltic pump pump speed 58r/min, height of observation 11.6mm, nebulizer pressure
0.23MPa, time of integration 15s.
Embodiment 2
The embodiment of the present invention provides a kind of a kind of inspection of elemental composition in vanadium chromium slag and its digestion procedure and measurement vanadium chromium slag
Survey method.
1, basic solvent is prepared
It is in powdered for taking natrium carbonicum calcinatum and boric acid to grind respectively, is 4 according to mass ratio：1 by natrium carbonicum calcinatum and boric acid
It is uniformly mixed and is placed in 110 DEG C of environment dry 1h.
2, it pre-oxidizes
Take respectively 0.20g vanadium chromium slag and 1.00g basic solvent be placed in platinum crucible be uniformly mixed be placed in Muffle furnace,
It is passed through air, is heated to 400 DEG C of reaction 15min.
3, frit reaction
Fusant is obtained after being continuously heating to 1000 DEG C of reaction 25min.
4, it dissolves by heating
It is cooled to room temperature to fusant, 30mL hydrochloric acid solution is added, be uniformly mixed, be placed in electric hot plate low-temperature heat to 97 DEG C
State close to boiling stops heating after fusant is completely dissolved, obtains lysate.
5, constant volume
Liquid to be dissolved is cooled to room temperature, and is diluted to volume in 500mL volumetric flask with deionized water and is uniformly mixed, vanadium chromium slag is made
Sample.
6, each element content in vanadium chromium slag is measured
Measure the content of the elements such as Si, Al, V, Ti, Cr, Na in vanadium chromium slag sample solution simultaneously using ICP-AES.Using
Directly the standard solution of each element to be measured is diluted with water be configured to concentration be 0.00%, 0.010%, 0.100%, 0.500%,
1.00%, the serial mixed standard solution of 8 of 5.00%, 10.0%, 15.0% is molten as no Matrix Match calibration curve standard
Liquid calibrates ICP-AES spectrometer with this and draws working curve.ICP-AES detection parameters, which are arranged, is：Analysis spectral line Si
251.611nm, Al 396.152nm, V 310.230nm, Ti 337.280nm, Cr 205.560nm, Na 589.592nm, RF
Power 1100W, secondary air speed 1.0L/min, peristaltic pump pump speed 58r/min, height of observation 11.6mm, nebulizer pressure
0.23MPa, time of integration 15s.
Embodiment 3
The embodiment of the present invention provides a kind of a kind of inspection of elemental composition in vanadium chromium slag and its digestion procedure and measurement vanadium chromium slag
Survey method.
1, basic solvent is prepared
It is in powdered for taking natrium carbonicum calcinatum and boric acid to grind respectively, is 4 according to mass ratio：1 by natrium carbonicum calcinatum and boric acid
It is uniformly mixed and is placed in 115 DEG C of environment dry 1.5h.
2, it pre-oxidizes
Take respectively 0.10g vanadium chromium slag and 0.50g basic solvent be placed in platinum crucible be uniformly mixed be placed in Muffle furnace,
It is passed through air, is heated to 300 DEG C of reaction 10min.
3, frit reaction
Fusant is obtained after being continuously heating to 950 DEG C of reaction 20min.
4, it dissolves by heating
It is cooled to room temperature to fusant, 25mL nitric acid solution is added, be uniformly mixed, be placed in electric hot plate low-temperature heat to 96 DEG C
State close to boiling stops heating after fusant is completely dissolved, obtains lysate.
5, constant volume
Liquid to be dissolved is cooled to room temperature, and is diluted to volume in 250mL volumetric flask with deionized water and is uniformly mixed, vanadium chromium slag is made
Sample.
6, each element content in vanadium chromium slag is measured
Measure the content of the elements such as Si, Al, V, Ti, Cr, Na in vanadium chromium slag sample solution simultaneously using ICP-AES.Using
Directly the standard solution of each element to be measured is diluted with water be configured to concentration be 0.00%, 0.010%, 0.100%, 0.500%,
1.00%, the serial mixed standard solution of 8 of 5.00%, 10.0%, 15.0% is molten as no Matrix Match calibration curve standard
Liquid calibrates ICP-AES spectrometer with this and draws working curve.ICP-AES detection parameters, which are arranged, is：Analysis spectral line Si
251.611nm, Al 396.152nm, V 310.230nm, Ti 337.280nm, Cr 205.560nm, Na 589.592nm, RF
Power 1100W, secondary air speed 1.0L/min, peristaltic pump pump speed 58r/min, height of observation 11.6mm, nebulizer pressure
0.23MPa, time of integration 15s.
Embodiment 4
The embodiment of the present invention provides a kind of a kind of inspection of elemental composition in vanadium chromium slag and its digestion procedure and measurement vanadium chromium slag
Survey method.
1, basic solvent is prepared
It is in powdered for taking natrium carbonicum calcinatum and boric acid to grind respectively, is 4 according to mass ratio：1 by natrium carbonicum calcinatum and boric acid
It is uniformly mixed and is placed in 120 DEG C of environment dry 1.5h.
2, it pre-oxidizes
Take respectively 0.20g vanadium chromium slag and 1.00g basic solvent be placed in platinum crucible be uniformly mixed be placed in Muffle furnace,
It is passed through air, is heated to 400 DEG C of reaction 15min.
3, frit reaction
Fusant is obtained after being continuously heating to 1000 DEG C of reaction 25min.
4, it dissolves by heating
It is cooled to room temperature to fusant, 30mL hydrochloric acid solution is added, be uniformly mixed, be placed in electric hot plate low-temperature heat to 95 DEG C
State close to boiling stops heating after fusant is completely dissolved, obtains lysate.
5, constant volume
Liquid to be dissolved is cooled to room temperature, and is diluted to volume in 500mL volumetric flask with deionized water and is uniformly mixed, vanadium chromium slag is made
Sample.
6, each element content in vanadium chromium slag is measured
Measure the content of the elements such as Si, Al, V, Ti, Cr, Na in vanadium chromium slag sample solution simultaneously using ICP-AES.Using
Directly the standard solution of each element to be measured is diluted with water be configured to concentration be 0.00%, 0.010%, 0.100%, 0.500%,
1.00%, the serial mixed standard solution of 8 of 5.00%, 10.0%, 15.0% is molten as no Matrix Match calibration curve standard
Liquid calibrates ICP-AES spectrometer with this and draws working curve.ICP-AES detection parameters, which are arranged, is：Analysis spectral line Si
251.611nm, Al 396.152nm, V 310.230nm, Ti 337.280nm, Cr 205.560nm, Na 589.592nm, RF
Power 1100W, secondary air speed 1.0L/min, peristaltic pump pump speed 58r/min, height of observation 11.6mm, nebulizer pressure
0.23MPa, time of integration 15s.
Precision assessment：
The digestion procedure that repetition carries out 8 independent vanadium chromium slags to Examples 1 to 4 respectively prepares vanadium chromium slag sample and measurement
Elemental composition in vanadium chromium slag, counts the average value and relative standard deviation (RSD) of 8 measurement structures respectively, and assesses this hair
The detection precision of the detection method of elemental composition is horizontal in the measurement vanadium chromium slag of bright offer, as shown in table 1：
1 Precision Experiment of table
As shown in Table 1, in measurement vanadium chromium slag provided by the invention in the detection method measurement vanadium chromium slag sample of elemental composition
When main amount and microelement, the relative standard deviation RSD of 1.0% or more content range of measurement result<1.0%, measurement result
The relative standard deviation RSD of 1.0% or less content range<5.0%, show that multiplicating measurement result is consistent, the repetition of method
Property, reproducibility it is good, method precision with higher is horizontal.
Accuracy evaluation：
The vanadium chromium slag each element compositional data that the embodiment of the present invention 1~4 detects is collected respectively.Then it is surveyed again using gravimetric method
Silicon, ammonium ferric sulfate or ferrous ammonium sulfate titration survey high-content vanadium-titanium-chromium, luminosity EDTA compleximetry surveys aluminium, diphenyl phosphinylidyne
Two hydrazine spectrophotometry survey trace chromium, tantalum reagent chloroform extraction spectrophotometry surveys trace vanadium, antimony molybdenum blue spectrophotometric method
Survey trace amounts of phosphorus, atomic absorption spectrography (AAS) (AAS) is surveyed the traditional analysis such as sodium and examined respectively to the vanadium chromium slag of Examples 1 to 4
Analysis is surveyed, by the check experiment of the methods of this method and classical chemical analysis, the sample to assess and verify this programme disappears
The accuracy of solution manufacturing method and its detection method is solved, as shown in table 2.
2 accuracy of table experiment
As shown in Table 2, the testing results control matrix such as this method and traditional classical chemical method is consistent, shows analysis knot
Fruit accuracy and reliability with higher.
In conclusion elemental composition in a kind of vanadium chromium slag provided by the invention and its digestion procedure and a kind of measurement vanadium chromium slag
Detection method, by optimization sample quality, basic solvent constitutes and dosage, dilution volume etc. between proportion relation, eliminate
The influence of sample matrices and basic solvent component to measurement, therefore calibration curve standard solution can direct gradient dilution element to be measured
Standard solution is prepared, without taking the interference corrections measure such as Matrix Match for carrying out sample matrices and flux component, significantly
Simplify the broad applicability of operating process and method application.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of digestion procedure of vanadium chromium slag is used for inductively coupled plasma atomic emission spectrometry detection elements ingredient,
It is characterized in that, the digestion procedure of the vanadium chromium slag includes：
Vanadium chromium slag and basic solvent mixed melting are obtained into fusant, acid solution is added after fusant is cooling and dissolves by heating.
2. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that mix vanadium chromium slag with basic solvent and melt
Melt including：
The powdered basic solvent and vanadium chromium slag are uniformly mixed, be warming up to 950~1000 DEG C of frit reactions 20~
25min；
Vanadium chromium slag and the basic solvent mass ratio are 1：5.
3. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that the basic solvent includes Carbon Dioxide
The mass ratio of sodium and boric acid, natrium carbonicum calcinatum described in the basic solvent and the boric acid is 4：1.
4. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that dissolving by heating fusant includes：
The acid solution is added in the fusant after cooling to be uniformly mixed, 95~97 DEG C are heated to, to the fusant
Stop heating after being completely dissolved.
5. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that the acid solution include dilute hydrochloric acid and
Any one in dust technology or two kinds；
The dilute hydrochloric acid is that the concentrated hydrochloric acid that mass percent concentration is 36~38% is matched according to 1 part of concentrated hydrochloric acid and 2 parts of deionized waters
It is made；
The dust technology is that the concentrated nitric acid that mass percent concentration is 65~68% is matched according to 1 part of concentrated nitric acid and 2 parts of deionized waters
It is made；
Acid solution described in 250~300mL is added in every gram of vanadium chromium slag.
6. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that before the mixed melting, need vanadium
Chromium slag carries out oxidation pre-treatment, and the oxidation pre-treatment includes：
The basic solvent and vanadium chromium slag are uniformly mixed, 300~400 DEG C of 10~15min of frit reaction are warming up to.
7. the digestion procedure of vanadium chromium slag according to claim 1, which is characterized in that after the heating for dissolving, need to carry out
Constant volume, the constant volume include：
It is cooled to room temperature to fusant lysate, with fusant lysate described in deionized water dilution constant volume；
The mass volume ratio of the vanadium chromium slag and the deionized water of constant volume is 0.3~0.5g/L.
8. a kind of vanadium chromium slag sample, which is characterized in that the vanadium chromium slag sample described in any item vanadium according to claim 1~7
The digestion procedure of chromium slag is cleared up to obtain.
9. the detection method of elemental composition in a kind of measurement vanadium chromium slag, which is characterized in that use inductively coupled plasma body atom
Transmitting spectrometry Simultaneous Direct Determination vanadium chromium slag sample according to any one of claims 8 in content be 0.01~15.0% Si, Al, V,
The content of Ti, Cr and Na element.
10. the detection method of elemental composition in measurement vanadium chromium slag according to claim 9, which is characterized in that calibration curve
Standard solution be directly diluted with water with the standard solution of each element to be measured be configured to concentration be respectively 0.00%~15.0% it is more
A mixed standard solution draws working curve calibration instrument with this.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696518A (en) * | 2018-12-20 | 2019-04-30 | 河钢股份有限公司承德分公司 | A kind of detection method of sub-molten salt vanadium extraction production tailings ingredient |
| CN110006736A (en) * | 2019-03-07 | 2019-07-12 | 江阴兴澄特种钢铁有限公司 | The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium |
| CN113686641A (en) * | 2021-09-07 | 2021-11-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for measuring aluminum content in silicon-calcium alloy |
| CN115876751A (en) * | 2023-02-06 | 2023-03-31 | 国能龙源环保有限公司 | Method for determining content of titanium-aluminum-calcium-magnesium-iron element in waste denitration catalyst through fluoride-free digestion |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
| CN106290318A (en) * | 2016-10-31 | 2017-01-04 | 云南磷化集团有限公司 | ICP AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously |
| CN106885800A (en) * | 2015-12-15 | 2017-06-23 | 云南冶金新立钛业有限公司 | The method drawn the working curve of sial calcium and magnesium manganese vanadium chromium in high titanium slag sample to be measured and determine wherein sial calcium and magnesium manganese vanadium chromium content |
| CN108414558A (en) * | 2018-03-20 | 2018-08-17 | 马鞍山钢铁股份有限公司 | A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method |
-
2018
- 2018-09-29 CN CN201811146528.4A patent/CN108872203A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
| CN106885800A (en) * | 2015-12-15 | 2017-06-23 | 云南冶金新立钛业有限公司 | The method drawn the working curve of sial calcium and magnesium manganese vanadium chromium in high titanium slag sample to be measured and determine wherein sial calcium and magnesium manganese vanadium chromium content |
| CN106290318A (en) * | 2016-10-31 | 2017-01-04 | 云南磷化集团有限公司 | ICP AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously |
| CN108414558A (en) * | 2018-03-20 | 2018-08-17 | 马鞍山钢铁股份有限公司 | A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method |
Non-Patent Citations (1)
| Title |
|---|
| 丁美英 等: "电感耦合等离子体原子发射光谱法测定炉渣中10种化学成分", 《冶金分析》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696518A (en) * | 2018-12-20 | 2019-04-30 | 河钢股份有限公司承德分公司 | A kind of detection method of sub-molten salt vanadium extraction production tailings ingredient |
| CN110006736A (en) * | 2019-03-07 | 2019-07-12 | 江阴兴澄特种钢铁有限公司 | The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium |
| CN113686641A (en) * | 2021-09-07 | 2021-11-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for measuring aluminum content in silicon-calcium alloy |
| CN115876751A (en) * | 2023-02-06 | 2023-03-31 | 国能龙源环保有限公司 | Method for determining content of titanium-aluminum-calcium-magnesium-iron element in waste denitration catalyst through fluoride-free digestion |
| 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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