CN106990098A - The method of each element content in simultaneous determination aluminium electrolyte - Google Patents
The method of each element content in simultaneous determination aluminium electrolyte Download PDFInfo
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Abstract
Each element content in a kind of simultaneous determination aluminium electrolyte, it is related to aluminum smelting technology chemical analysis field, this method determines the emitted luminescence intensity of the standard liquid of multiple different solutions concentration of each element using inductive coupling plasma emission spectrograph first, standard curve is drawn, secondly by the melting of aluminium electrolyte sample mixing potassium pyrosulfate, cooling, hydrochloric acid and water extraction is used, obtain sample solution, potassium pyrosulfate is melted, cooled down, using hydrochloric acid and water extraction, blank reagent is obtained；Then the emitted luminescence intensity of sample solution and the emitted luminescence intensity of blank test solution are determined, detectable concentration and blank concentration are checked in by standard curve, the mass concentration of each element in aluminium electrolyte sample is finally calculated.This method utilizes inductively coupled plasma atomic emission spectrometry, realizes the content of Al, Na, Ca, Mg, Li each element in quick, easy, accurate simultaneous determination aluminium electrolyte, and this method is workable, analysis cost is low.
Description
Technical field
The present invention relates to a kind of aluminum smelting technology chemical analysis field, and Al in more particularly to a kind of simultaneous determination aluminium electrolyte,
The method of Na, Ca, Mg, Li each element content.
Background technology
Aluminium electrolyte is the core of aluminium metallurgy, and its position is between anode and negative electrode.Electrolytic bath is usual
Containing ice crystal, aluminum oxide, and additive aluminum fluoride, calcirm-fluoride, magnesium fluoride and lithium fluoride etc..Wherein, ice crystal and fluorination
Aluminium is flux, and aluminum oxide is the raw material of aluminium metallurgy, and other fluorination salt additives are used for the quality and current efficiency for ensureing aluminium, and improve
The physicochemical properties of cryolite-alumina liquation, for example, reduce its fusing point, or improves its conductance, reduces the dissolving of aluminium
Degree etc..But, the addition of additive makes the composition of aluminium electrolyte become complicated, and Al, Na, Ca, Mg, Li element turn into aluminium electrolyte
In important composition element.Determining each element content in electrolyte fused solution can be as the necessity for controlling constituent content in electrolyte
Detection means, that is to say, that if containing for Al, Na, Ca, Mg, Li each element in aluminium electrolyte can quickly and accurately be analyzed
Amount, the addition of various additives in aluminium electrolyte just can be adjusted in time.Therefore, to each element content in electrolyte fused solution
Measure specification it is more necessary, it has important theory significance and application value to aluminum smelting industry.
Mainly there are titration, atomic absorption spectrography (AAS) etc. currently used for the chemical method for determining constituent content in aluminium electrolyte,
But analyzing purity complex steps, efficiency is low, and time-consuming；Atomic absorption spectrography (AAS) can only be individually measured to each element,
Analysis time is longer, and the range of linearity is narrow.Have to the specific standards that the constituent content in aluminium electrolyte is detected：YS/T739《Aluminium
The measure x ray fluorescence spectrometry of electrolyte molecule when main component》Be in present analysis aluminium electrolyte constituent content and point
The method of sub- ratio, though the method analyze speed is fast, batch chemically examines the requirement of main component in aluminium electrolyte when meeting production.But
It is when this method determines the main component in aluminium electrolyte using Xray fluorescence spectrometer, curves shift often to occur, causes
The inaccurate phenomenon of measurement result；And can only analyze calcium fluoride containing CaF using this method2, magnesium fluoride MgF2Two kinds of fluoride salt additions
The aluminium electrolyte of agent, when chemically examining containing the more complicated aluminium electrolyte of composition, it may appear that analysis result is inaccurate, and with a low credibility shows
As.YS/T768《The measure flame atomic absorption spectrometry of lithium content in aluminium electrolyte》It is to analyze the Li contents in electrolyte
Analysis in method, but the standard not to other elements such as Na, Ca, Mg.
Accordingly, it would be desirable to which one kind can realize Al, Na, Ca, Mg, Li in quick, easy, accurate simultaneous determination aluminium electrolyte
The method of each element content.
The content of the invention
It is an object of the invention to provide a kind of method of each element content in simultaneous determination aluminium electrolyte, it utilizes inductance
Coupled plasma-atomic emission spectrometry, realize Al in quick, easy, accurate simultaneous determination aluminium electrolyte, Na, Ca, Mg,
The content of Li each elements, this method is workable, analysis cost is low.
The present invention is solved its technical problem and realized using following technical scheme.
The method that the present invention proposes each element content in a kind of simultaneous determination aluminium electrolyte, it comprises the following steps：
Multiple differences of each element in Al, Na, Ca, Mg, Li are determined using inductive coupling plasma emission spectrograph
Emitted luminescence intensity of the standard liquid of solution concentration under the optimized analysis spectral line of corresponding element, and draw Al, Na, Ca, Mg, Li
In each element solution concentration and emitted luminescence intensity between standard curve, wherein, potassium pyrosulfate is also contained in standard liquid
And hydrochloric acid；
Aluminium electrolyte sample mixing potassium pyrosulfate is heated to molten condition, cooling, hydrochloric acid is reused and water is leached,
And sample solution is made；Potassium pyrosulfate is heated to molten condition, cooling, hydrochloric acid is reused and water is leached, and sky is made
Potassium pyrosulfate, the concentration of hydrochloric acid in potassium pyrosulfate, the concentration of hydrochloric acid and standard liquid in white reagent, blank reagent and sample solution
Correspondent equal；
Using inductive coupling plasma emission spectrograph, determine respectively sample solution and blank reagent Al, Na, Ca,
Emitted luminescence intensity under the optimized analysis spectral line of each element in Mg, Li, and according to standard curve obtain Al, Na, Ca, Mg,
The detectable concentration and blank concentration of each element in Li；
The aluminium electroloysis of the detectable concentration of each element in Al, Na, Ca, Mg, Li, blank concentration and sample solution
Quality sample concentration calculates the mass concentration of each element to be measured in aluminium electrolyte sample.
Further, in present pre-ferred embodiments, according to below equation, each member to be measured in aluminium electrolyte sample is calculated
The mass concentration w (x) of element：Wherein, c is the inspection of element to be measured
Survey concentration, c0For the blank concentration of element to be measured, V is the volume of sample solution, and R is multiple different solutions concentration of element to be measured
Standard liquid the coefficient of dilution, m0For the quality of aluminium electrolyte sample.
Further, in present pre-ferred embodiments, m0=0.1000~0.5000g.
Further, in present pre-ferred embodiments, the preparation method of aluminium electrolyte sample is：By aluminium electroloysis mass mistake
0.074mm standard screens, in 100~110 DEG C of drying, are transferred in drier and are cooled to room temperature.
Further, in present pre-ferred embodiments, the method for aluminium electrolyte sample mixing potassium pyrosulfate heating is：First
Aluminium electrolyte sample is placed in platinum ware, potassium pyrosulfate is added, is placed on electric hot plate and is heated to fusing, be transferred to high-temperature box type
Melted in resistance furnace, melting temperature is 700~750 DEG C, the melting time is 20~30min.
Further, in present pre-ferred embodiments, the method for leaching is：Hydrochloric acid and hot water are added into platinum ware, plus
Heat to sample is completely dissolved.
Further, in present pre-ferred embodiments, first according to preparing blank reagent identical method, preparation is obtained
Matrix Solution, reuses the standard that Matrix Solution prepares the multiple different solutions concentration for obtaining blank reagent and each element respectively
Solution.
Further, in present pre-ferred embodiments, Al optimized analysis spectral line is 396.152nm, optimal point of Na
Analysis spectral line is 588.995nm and 589.592nm, Ca optimized analysis spectral line are 317.933nm, and Mg optimized analysis spectral line is
285.213nm, Li optimized analysis spectral line are 670.784nm.
Further, in present pre-ferred embodiments, in aluminium electrolyte sample, Al measurement range for 10%~
The measurement range that the measurement range that 20%, Na measurement range are 20%~35%, Ca is 0.5%~10%, Mg is 0.1%~
5%, Li measurement range are 0.05%~5%.
Further, in present pre-ferred embodiments, potassium pyrosulfate in sample solution, blank reagent and standard liquid
Mass-volume concentration is 10~15mg/mL, and the concentration of volume percent of hydrochloric acid is 3%~3.5%.
The beneficial effect of the method for each element content is in the simultaneous determination aluminium electrolyte of the embodiment of the present invention：This method is first
The transmitting of the standard liquid of multiple different solutions concentration of each element is first determined using inductive coupling plasma emission spectrograph
Luminous intensity, draws standard curve, secondly by the melting of aluminium electrolyte sample mixing potassium pyrosulfate, cooling, using hydrochloric acid and water extraction,
Sample solution is obtained, potassium pyrosulfate is melted, cooled down, using hydrochloric acid and water extraction, blank reagent is obtained；Then sample is determined molten
The emitted luminescence intensity of liquid and the emitted luminescence intensity of blank test solution, check in detectable concentration and blank concentration, finally by standard curve
Calculate the mass concentration of each element in aluminium electrolyte sample.This method utilizes inductively coupled plasma atomic emission spectrometry,
The relative standard deviation measurement range of each element is 0.05%~1.12%, and the degree of accuracy is higher, and stability is good, precision is high,
The content of Al, Na, Ca, Mg, Li each element in quick, easy, accurate simultaneous determination aluminium electrolyte is realized, this method is operable
Property strong, analysis cost it is low, available for standard sample and production sample analysis.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
The method to each element content in the simultaneous determination aluminium electrolyte of the embodiment of the present invention is specifically described below.
The method that the embodiment of the present invention provides each element content in a kind of simultaneous determination aluminium electrolyte, it utilizes inductive
The content of Al, Na, Ca, Mg, Li each element in plasma emlssion spectrometry, simultaneous determination aluminium electrolyte, wherein, Al measurement
The measurement range that scope is 10%~20%, Na is that 20%~35%, Ca measurement range is 0.5%~10%, Mg measurement
The measurement range that scope is 0.1%~5%, Li is 0.05%~5%.This method specifically includes following steps：
(1) series standard solution is configured：Multiple different solutions of each element in Al, Na, Ca, Mg, Li are prepared respectively
Also contain potassium pyrosulfate and hydrochloric acid in the standard liquid of concentration, i.e. series standard solution, standard liquid.It is each in the present embodiment
The series standard solution for planting element is preferably diluted the typical shelf solution of the element according to coefficient of dilution R step by step, respectively
The concentration of the typical shelf solution of element is 1.0mg/mL, is easy to be configured to the standard liquid of variant solution concentration；Standard is molten
The mass-volume concentration of potassium pyrosulfate is 10~15mg/mL in liquid, and the concentration of volume percent of hydrochloric acid is 3%~3.5%.
(2) standard curve is drawn：
First, composed according to the optimized analysis of each element in composition selection Al, Na, Ca, Mg, Li of aluminium electrolyte sample
Line, exists very big dry because using different analysis spectral lines, the result determined differs greatly, between analysis spectral line
Disturb, not only exist between the different analysis spectral lines of same element and disturb, and there is also very big between the analysis spectral line of different elements
Interference, while the intensity of different analysis spectral line is also different.So the present invention is screened to each element analysis spectral line,
In the present embodiment, Al optimized analysis spectral line is 396.152nm, Na optimized analysis spectral line for 588.995nm and
589.592nm, Ca optimized analysis spectral line are 317.933nm, and Mg optimized analysis spectral line is 285.213nm, optimal point of Li
Analysis spectral line is 670.784nm.
Then, each in above-mentioned Al, Na, Ca, Mg, Li is determined respectively using inductive coupling plasma emission spectrograph
Emitted luminescence intensity of the standard liquid of element under the optimized analysis spectral line of corresponding element, is specifically that standard liquid is passed through into sample introduction
System is introduced into inductive coupling plasma emission spectrograph and detected, and draws the element of each in Al, Na, Ca, Mg, Li
Solution concentration and emitted luminescence intensity between standard curve.
(3) sample solution is prepared：
First, pre-treatment is carried out to aluminium electroloysis mass：By the sieving of aluminium electroloysis mass, drying, cooling, 0.074mm is preferably crossed
Standard screen, in 100~110 DEG C of drying in oven, is transferred in drier and is cooled to after room temperature, obtain aluminium electrolyte sample.
Then, quality m is weighed0=0.1000~0.5000g aluminium electrolyte sample mixing potassium pyrosulfate is heated to melting
State, cooling, reuse hydrochloric acid and water is leached, until sample is completely dissolved, and are made burnt in sample solution, sample solution
Potassium pyrosulfate in the concentration correspondent equal of potassium pyrosulfate, hydrochloric acid, the sample solution in potassium sulfate, the concentration of hydrochloric acid and standard liquid
Mass-volume concentration be 10~15mg/mL, the concentration of volume percent of hydrochloric acid is 3%~3.5%.Wherein, aluminium electrolyte sample
Product mixing potassium pyrosulfate heating method be：First aluminium electrolyte sample is placed in digestion device platinum ware, it is burnt then at adding at room temperature
Potassium sulfate, be placed on electric hot plate be heated to fusing, be then transferred in high temperature box type resistance furnace melt, melting temperature be 700~
750 DEG C, the melting time is 20~30min, and taking-up is cooled to room temperature.The method of leaching is：Hydrochloric acid and hot water are added into platinum ware,
And be heated to sample and be completely dissolved, preferably leaching liquid is transferred in igelite beaker after leaching and cooled down；Again plus hydrochloric acid
Leachate is diluted with water, volume is settled to for V, obtains sample solution.
(4) blank reagent is configured, according to preparing sample solution identical method, potassium pyrosulfate is heated to molten
State, cooling, reuse hydrochloric acid and water is leached, and blank reagent is made, in blank reagent potassium pyrosulfate, the concentration of hydrochloric acid with
The mass-volume concentration of potassium pyrosulfate is 10 in the concentration correspondent equal of potassium pyrosulfate, hydrochloric acid, the blank reagent in standard liquid
~15mg/mL, the concentration of volume percent of hydrochloric acid is 3%~3.5%.
In the present embodiment, in order to ensure the concentration of the potassium pyrosulfate in sample solution, blank reagent and standard liquid, hydrochloric acid
It is equal, can be first according to preparing blank reagent identical method, preparation obtains Matrix Solution, reuses Matrix Solution and match somebody with somebody respectively
The standard liquid of blank reagent and multiple different solutions concentration of each element is made.
(5) sample solution is detected：Using inductive coupling plasma emission spectrograph, what difference determination step (3) was prepared
Emitted luminescence intensity under the optimized analysis spectral line of each element of the sample solution in Al, Na, Ca, Mg, Li, and according to corresponding element
The standard curve of element checks in detectable concentration for c；The blank test solution that determination step (4) is prepared respectively is in Al, Na, Ca, Mg, Li
Emitted luminescence intensity under the optimized analysis spectral line of each element, and blank concentration is checked according to the standard curve of corresponding element be
c0。
Inductively coupled plasma atomic absorption spectrography (AAS) has sensitivity height, precision good due to it, without chemistry point
From single injected sampling just can determine multiple element simultaneously, and standard curve range is wide, the advantages of test speed is fast, be widely used in each
The analysis of material composition is planted, there is good application prospect.Inductive coupling plasma emission spectrograph used in the present invention is
IRIS1000 types Induction Couple Plasma (U.S.'s thermoelectricity), inductively coupled plasma transmitting
The condition of work of spectrometer is：RF power is 1150W, and assistor flow is 0.5L/min, and pump speed is 80~130r/min, atomization
Device flow is 0.65L/min, and the time of integration is 15s.
(6) each element content is calculated：The detectable concentration, the sky of each element in Al, Na, Ca, Mg, Li
The aluminium electrolyte sample concentration of white concentration and the sample solution calculates each element to be measured in the aluminium electrolyte sample
Mass concentration.It is preferred that according to below equation, calculating the mass concentration w (x) of each element to be measured in the aluminium electrolyte sample：Wherein, c is the detectable concentration of element to be measured, c0For member to be measured
The blank concentration of element, V is the volume of sample solution, and R is the dilution of the standard liquid of multiple different solutions concentration of element to be measured
Coefficient, m0For the quality of aluminium electrolyte sample.
The feature and performance to the present invention are described in further detail with reference to embodiments.
Instrument equipment and condition of work are tested in the embodiment of the present invention：
IRIS1000 types Induction Couple Plasma (U.S.'s thermoelectricity), condition of work：RF work(
Rate is 1150W, and assistor flow is 0.5L/min, and pump speed is 80~130r/min, and nebulizer flow is 0.65L/min, integration
Time is 15s；250mL polytetrafluoroethylene beakers, are handled through nitric acid dousing, it is desirable to which temperature in use is less than 200 DEG C；Electronic balance,
Sensibility reciprocal 0.1mg；Electric hot plate；High temperature box type resistance furnace, it is 700~750 DEG C to control temperature.
Main agents are tested in the embodiment of the present invention：
Potassium pyrosulfate, top pure grade；Hydrochloric acid (1+1), top pure grade；Sodium hydroxide, top pure grade；Metallic aluminium (Al >=99.99%)；
Sodium chloride (standard reagent)；Calcium carbonate (standard reagent)；Magnesium metal (Mg >=99.99%)；Lithium carbonate (standard reagent)；Experiment is used
Water is laboratory one-level water.
Embodiment 1
The method that embodiment 1 provides each element content in a kind of simultaneous determination aluminium electrolyte, this method utilizes inductive
Plasma emission spectrometer, joint-detection, aluminium electroloysis are carried out to Al, Na, Ca, Mg, Li constituent content in aluminium electrolyte sample
Quality sample selects the aluminium electrolyte standard specimen GDJ-1 that Zhengzhou Inst of Light Metals is produced, and this method specifically includes following steps：
10g potassium pyrosulfates are weighed in platinum ware, is placed on electric hot plate and is heated to fusing, then move into high temperature box type resistance furnace
In in 725 DEG C melt about 25min, taking-up be cooled to room temperature；Added in fused mass into platinum ware by 10mL hydrochloric acid and appropriate heat
Water extraction, is heated to sample and is completely dissolved, and moves into 250mL vinyon beakers, 200mL volumetric flasks are transferred to after cooling
In, scale is diluted with water to, mixes, obtains Matrix Solution, the mass-volume concentration of potassium pyrosulfate is 50mg/ in the Matrix Solution
ML, the concentration of volume percent of hydrochloric acid is 5%.
Compound concentration is the typical shelf solution of 1.0mg/mL Al, Na, Ca, Mg, Li each element：
A. sodium typical shelf solution：It is accurate weigh 2.540g sodium chloride (in advance prior to 500 DEG C~600 DEG C calcinations to constant weight) in
In 400mL beakers, the dissolving of 20mL hydrochloric acid low-grade fever is added.Cooling, solution is moved into 1000mLPFA volumetric flasks, is diluted to water
Scale, is mixed, this solution 1mL sodium containing 1.0mg.
B. standard calcium stock solution：It is accurate to weigh the pre- calcium carbonate prior to 105 DEG C of drying of 2.4971g, it is placed in beaker, covers
Upper table ware, adds 10mL water, hydrochloric acid is added dropwise to being completely dissolved, 20mL hydrochloric acid is added, boils removing carbon dioxide, removes
Cooling, moves into 1000mL volumetric flasks, is diluted with water to scale, shakes up, this solution 1mL calcium containing 1.0mg.
C. magnesium typical shelf solution：1.0000g magnesium metals accurately are weighed, are placed in 400mL beakers, 40mL hydrochloric acid is added,
Table ware is covered, is slowly heated to be completely dissolved, is cooled down, solution is moved into 1000mL volumetric flasks, scale is diluted with water to, is mixed
It is even, this solution 1mL magnesium containing 1.0mg.
D. lithium typical shelf solution：The accurate 5.3228g lithium carbonates that weigh are (in advance in 280 DEG C of ± 10 DEG C of drying 2h and dry
Room temperature is cooled in dry device), it is placed in 200mL beakers, plus 20mL dissolving with hydrochloric acid, carbon dioxide is driven away in heating, after cooling
People's 1000mI volumetric flasks are moved, scale is diluted with water to, shakes up, this solution 1mL contains 1.0mg lithiums.
E. aluminium typical shelf solution：Accurately weigh 1.0000g metallic aluminiums in polytetrafluoroethylene beaker, add 20mL water and
3g sodium hydroxides, make after it is completely dissolved, to be slowly neutralized to and precipitated with hydrochloric acid, and excessive 20mL, and heating dissolves it, cold
But, move into 1000mL volumetric flasks, be diluted with water to scale, shake up, this solution 1mL aluminium containing 1.0mg.
Typical shelf solution is diluted step by step according to coefficient of dilution R using Matrix Solution and water, is specifically to move respectively
The typical shelf solution of different amounts of above-mentioned each element is taken, one group of 100mL volumetric flask for being previously added 25mL Matrix Solutions is placed in
In, 2mL hydrochloric acid is added, scale is diluted with water to, mixed, obtains burnt in the series standard solution of each element, series standard solution
The mass-volume concentration of potassium sulfate is 12.5mg/mL, and the concentration of volume percent of hydrochloric acid is 3.25%；The series standard of each element
Constituent content should be within the scope of its corresponding working curve in solution, and the quantity of series standard solution is determined by required precision,
The series standard solution of every kind of element at least includes 6 different standard liquids.
According to the optimized analysis spectral line of the composition selection each element of aluminium electrolyte sample, the recommendation optimized analysis spectrum of each element
Line is as follows：
The recommendation optimized analysis spectral line of each element of table 1
| Element | Analytical line/nm |
| Al | 396.152 |
| Na | 588.995、589.592 |
| Ca | 317.933 |
| Mg | 285.213 |
| Li | 670.784 |
The series standard solution prepared is introduced into inductive coupling plasma emission spectrograph by sampling system
Row detection, determines emitted luminescence intensity of the series standard solution of each element under the optimized analysis spectral line of the element, draws each member
Standard curve between the concentration and emitted luminescence intensity of element, respectively obtains Al, Na, Ca, Mg, Li standard curve.
After aluminium electrolyte sample is ground, 0.074mm standard screens are crossed, prior to 100~110 DEG C drying in oven are retransferred
Room temperature is cooled into drier；Weigh quality m0=0.2g above-mentioned aluminium electrolyte sample, is accurate to 0.0001g, is placed in platinum
In ware, 5g potassium pyrosulfates are added at room temperature and are mixed, is placed on electric hot plate and is heated to fusing, then move into high temperature box type resistance furnace
In melt about 25min in 725 DEG C, until going fluorine removal completely, taking-up is cooled to room temperature；5mL is added in fused mass into platinum ware
Hydrochloric acid and the leaching of 30mL hot water, are heated to being completely dissolved；Leaching liquid is transferred in 250mL igelite beakers, cooled down,
Move into 200mL volumetric flasks, be diluted with water to scale, mix, obtain test solution；Divide and take the above-mentioned test solutions of 50mL in 100mL volumetric flasks,
2mL hydrochloric acid is added, scale is diluted with water to, mixes, obtains sample solution, the quality volume of potassium pyrosulfate is dense in the sample solution
Spend for 12.5mg/mL, the concentration of volume percent of hydrochloric acid is 3.25%.
Take 25mL Matrix Solutions to add in 100mL volumetric flasks, add 2mL hydrochloric acid, be diluted with water to scale, mix, obtain
The mass-volume concentration of potassium pyrosulfate is 12.5mg/mL in blank reagent, the blank reagent, and the concentration of volume percent of hydrochloric acid is
3.25%.
When the linearly dependent coefficient >=0.999 of working curve, sample solution is introduced into inductive by sampling system
Plasma emission spectrometer, determines emitted luminescence intensity of the sample solution under the optimized analysis spectral line of element to be measured, and treating
Detectable concentration is checked on the standard curve for surveying element for c；Blank test solution is introduced into measure blank test solution by sampling system to treat
The emitted luminescence intensity surveyed under the optimized analysis spectral line of element, and blank concentration is checked in for c on the standard curve of element to be measured0。
Calculate the mass percent concentration of element to be measured in aluminium electrolyte sample
Up to the mass concentration of Al, Na, Ca, Mg, Li in measure and calculation aluminium electrolyte sample respectively.
Embodiment 2
The method that embodiment 2 provides each element content in a kind of simultaneous determination aluminium electrolyte, aluminium electrolyte sample selects Zheng
The aluminium electrolyte standard specimen GDJ-2 of state light metal research institute production, this method is identical with the method in embodiment 1.
Embodiment 3
The method that embodiment 3 provides each element content in a kind of simultaneous determination aluminium electrolyte, aluminium electrolyte sample selects Zheng
The aluminium electrolyte standard specimen GDJ-3 of state light metal research institute production, this method is roughly the same with the method in embodiment 1, difference
Be in：Melting temperature is 700 DEG C, and the melting time is 30min；Potassium pyrosulfate in sample solution, blank reagent and standard liquid
Mass-volume concentration be 10mg/mL, the concentration of volume percent of hydrochloric acid is 3%.
Embodiment 4
The method that embodiment 4 provides each element content in a kind of simultaneous determination aluminium electrolyte, aluminium electrolyte sample selects Zheng
The aluminium electrolyte standard specimen GDJ-4 of state light metal research institute production, this method is identical with the method in embodiment 3.
Embodiment 5
The method that embodiment 5 provides each element content in a kind of simultaneous determination aluminium electrolyte, aluminium electrolyte sample selects Zheng
The aluminium electrolyte standard specimen GDJ-5 of state light metal research institute production, this method is roughly the same with the method in embodiment 1, difference
Be in：Melting temperature is 750 DEG C, and the melting time is 20min；Potassium pyrosulfate in sample solution, blank reagent and standard liquid
Mass-volume concentration be 15mg/mL, the concentration of volume percent of hydrochloric acid is 3.5%.
Embodiment 6
The method that embodiment 6 provides each element content in a kind of simultaneous determination aluminium electrolyte, aluminium electrolyte sample selects Zheng
The aluminium electrolyte standard specimen GDJ-6 of state light metal research institute production, this method is identical with the method in embodiment 5.
The degree of accuracy and precision to embodiment 1-6 are tested：
The concrete content of each aluminium electrolyte standard specimen in embodiment 1-6 is as shown in table 2：
The each element content of the aluminium electrolyte standard specimen of table 2
A. precision test：Using 6 aluminium electrolyte standard specimens of Zhengzhou Inst of Light Metals, each aluminium electrolyte standard specimen
6 parallel determinations, the relative standard deviation to each aluminium electrolyte standard specimen is evaluated, 1-6 of embodiment of the present invention inspection
The precision result of survey method is as shown in table 3.
The Precision test result of table 3
It was found from the measurement result of table 3, the relative standard deviation scopes of 6 parallel determinations of Al elements for 0.12%~
0.33%；The relative standard deviation scope of Na elements is 0.05%~0.24%；The relative standard deviation scope of Ca elements is
0.50%~1.12%；The relative standard deviation scope of Mg elements is 0.43%~0.86%；The relative standard deviation of Li elements
Scope is 0.39%~0.94%.The standard deviation of above-mentioned element is completely in national standard error range, therefore, detection of the invention
The method degree of accuracy can meet actual analysis needs.
B. accuracy test：Pass through the rate of recovery of 6 aluminium electrolyte standard specimen measurement results to Zhengzhou Inst of Light Metals
To evaluate the degree of accuracy of detection method, result of the test is as shown in table 4.
The recovery test result of table 4
From the detection data in table 4 can be seen that using the present invention detection method simultaneous determination aluminium electrolyte in Al,
During five kinds of constituent contents of Na, Ca, Mg, Li, rate of recovery scope is 96.40%~102.35%, and above-mentioned five can be determined exactly
The content of element is planted, further proving the detection method of the present invention has the very high degree of accuracy.
In summary, in the simultaneous determination aluminium electrolyte of the embodiment of the present invention each element content method, it utilizes inductance
Coupled plasma-atomic emission spectrometry, realize Al in quick, easy, accurate simultaneous determination aluminium electrolyte, Na, Ca, Mg,
The content of Li each elements, this method is workable, analysis cost is low.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of method of each element content in simultaneous determination aluminium electrolyte, it is characterised in that it comprises the following steps：
Multiple different solutions of each element in Al, Na, Ca, Mg, Li are determined using inductive coupling plasma emission spectrograph
Emitted luminescence intensity of the standard liquid of concentration under the optimized analysis spectral line of the correspondence element, and draw Al, Na, Ca, Mg, Li
In each element solution concentration and emitted luminescence intensity between standard curve, wherein, also containing burnt sulphur in the standard liquid
Sour potassium and hydrochloric acid；
Aluminium electrolyte sample mixing potassium pyrosulfate is heated to molten condition, cooling, hydrochloric acid is reused and water is leached, and make
Obtain sample solution；Potassium pyrosulfate is heated to molten condition, cooling, hydrochloric acid is reused and water is leached, and blank examination is made
Potassium pyrosulfate, the concentration of hydrochloric acid and potassium pyrosulfate, salt in the standard liquid in agent, the blank reagent and the sample solution
The concentration correspondent equal of acid；
Using inductive coupling plasma emission spectrograph, determine respectively the sample solution and the blank reagent Al, Na,
Emitted luminescence intensity under the optimized analysis spectral line of each element in Ca, Mg, Li, and according to the standard curve obtain Al, Na,
The detectable concentration and blank concentration of each element in Ca, Mg, Li；
The detectable concentration of each element in Al, Na, Ca, Mg, Li, the blank concentration and the sample solution
Aluminium electrolyte sample concentration calculate the mass concentration of each element to be measured in the aluminium electrolyte sample.
2. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that
According to below equation, the mass concentration w (x) of each element to be measured in the aluminium electrolyte sample is calculated：Wherein, c is the detectable concentration of element to be measured, c0For member to be measured
The blank concentration of element, V is the volume of sample solution, and R is the dilution of the standard liquid of multiple different solutions concentration of element to be measured
Coefficient, m0For the quality of aluminium electrolyte sample.
3. the method for each element content in simultaneous determination aluminium electrolyte according to claim 2, it is characterised in that m0=
0.1000~0.5000g.
4. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that the aluminium
The preparation method of electrolyte sample is：Aluminium electroloysis mass is crossed into 0.074mm standard screens, in 100~110 DEG C of drying, is transferred to dry
Room temperature is cooled in dry device.
5. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that the aluminium
Electrolyte sample mixing potassium pyrosulfate heating method be：First aluminium electrolyte sample is placed in platinum ware, the burnt sulphur is added
Sour potassium, is placed on electric hot plate and is heated to fusing, is transferred in high temperature box type resistance furnace and melts, and the melting temperature is 700~750
DEG C, the melting time is 20~30min.
6. the method for each element content in simultaneous determination aluminium electrolyte according to claim 5, it is characterised in that the leaching
The method taken is：Hydrochloric acid and hot water are added into the platinum ware, the sample is heated to and is completely dissolved.
7. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that first according to
With preparing the blank reagent identical method, preparation obtains Matrix Solution, reuses Matrix Solution and prepares respectively and obtains described
The standard liquid of blank reagent and multiple different solutions concentration of each element.
8. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that Al is most
Good analysis spectral line is 396.152nm, and Na optimized analysis spectral line is 588.995nm and 589.592nm, Ca optimized analysis spectral line
For 317.933nm, Mg optimized analysis spectral line is 285.213nm, and Li optimized analysis spectral line is 670.784nm.
9. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that the aluminium
In electrolyte sample, the measurement range that the measurement range that Al measurement range is 10%~20%, Na is 20%~35%, Ca is
The measurement range that 0.5%~10%, Mg measurement range are 0.1%~5%, Li is 0.05%~5%.
10. the method for each element content in simultaneous determination aluminium electrolyte according to claim 1, it is characterised in that described
The mass-volume concentration of potassium pyrosulfate is 10~15mg/mL, salt in sample solution, the blank reagent and the standard liquid
The concentration of volume percent of acid is 3%~3.5%.
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