CN110057810A - Clear up vanadium titanium blast furnace gas mud/ash method and detection method - Google Patents
Clear up vanadium titanium blast furnace gas mud/ash method and detection method Download PDFInfo
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- CN110057810A CN110057810A CN201910409595.9A CN201910409595A CN110057810A CN 110057810 A CN110057810 A CN 110057810A CN 201910409595 A CN201910409595 A CN 201910409595A CN 110057810 A CN110057810 A CN 110057810A
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Abstract
The invention belongs to test and analyze technical field, and in particular to resolution vanadium titanium blast furnace gas mud/ash method and detection method.The present invention clears up vanadium titanium blast furnace gas mud/ash method the following steps are included: weighing vanadium titanium blast furnace gas mud/ash sample, first it is placed in calcination in high temperature furnace, then water, hydrofluoric acid, chloroazotic acid are reused and carries out heating resolution reaction, sulfuric acid is added, and the reaction was continued to the sulfuric acid decomposition generation dense white cigarette mist of sulfur trioxide, the reaction of concentrated nitric acid Strong oxdiative is added dropwise, continue heating reaction to the dense white cigarette mist of sulfur trioxide is generated again, adds water and nitric acid dissolved salts；Constant volume is diluted with water after cooling, to obtain detecting sample solution used.The method of the present invention can clear up vanadium titanium blast furnace gas mud/ash well, to ensure that the accuracy of testing result.
Description
Technical field
The invention belongs to test and analyze technical field, and in particular to a kind of resolution vanadium titanium blast furnace gas mud/ash method with
And the method for detecting the Determination of Rare-Expensive Elements content such as In, Sc, Ge, Ga, Sr, Zr, Co in vanadium titanium blast furnace gas mud/ash.
Background technique
China's Panxi Diqu, which is contained, the huge multielement of reserves (companion) raw v-ti magnetite ore resources altogether, and only branch is climbed in Sichuan
Spend within the border existing explored reserves be as high as 73.37 hundred million tons, resource features are not only containing the major metals such as iron, titanium, vanadium member
Element, but also dilute scattered precious metal element of the high value containing there are many coexists, although since many precious metal elements are in primary ore deposit
Content is lower in resource and is influenced by occurrence patterns and is directly utilized with being difficult to economical and efficient, but in existing refinement v-ti magnetite
In mine in the process flow of ferrotitanium vanadium, rare and scatter element is enriched in certain process links by deposition to a certain degree, contents level phase
It is relatively easy to increase and substrate medium, therefore have recycling value and condition.
Wherein, during using vanadium titano-magnetite blast furnace ironmaking, the impurity such as lead, zinc, indium for being coexisted in magnetic iron ore
Component is reduced, and forms steam in high-temperature region, with blast furnace coal together with the fine solid particle of the substances such as ore, coke and flux
Gas, which is carried, comes out of the stove outside, is captured and is collected by dust separation system, usually claimed by the obtained dry type fine-grained powder of dry dust removal mode
Meaning gas ash, the product obtained by wet dust removal mode is just referred to as meaning gas mud through precipitation process sludge obtained.Vanadium titanium
In blast furnace gas mud (ash) in addition to containing elements such as more iron, carbon, zinc, lead, titanium, calcium, magnesium, phosphorus, also has and be enriched to
The Determination of Rare-Expensive Elements such as indium, scandium, germanium, gallium, strontium, zirconium, cobalt of suitable contents level, these elements usually with polycompound or
The forms such as carbide exist, and vanadium titano-magnetite comprehensive utilization of resources requires exploitation related process technologies sufficiently, efficiently, economically to return
Receive these Determination of Rare-Expensive Elements.It is dilute scattered to need accurately to grasp In, Sc, Ge, Ga, Sr, Zr, Co etc. in vanadium titanium blast furnace gas mud thus
The content of element provides detection technique branch using the technology of rare and scatter element to develop the resource utilization from solid waste
Support.
The associated prior art mainly use hydrochloric acid, nitration acid heat dissolution ore class sample, then with crystallization or
The extraction measurements such as spectroscopic methodology and polarography, which are pluged with molten metal, waits elements, and such analysis method is not only difficult to be cleared up quick and completely containing a large amount of
The gas mud sample of free carbon and copmbined-carbon, the real content that can not accurately grasp your dilute element in gas mud is horizontal, influences dilute
Exploitation, actual production control and the calculating of element recovery rate of your element extraction technology etc., and there are complicated for operation numerous
Trivial, round of visits long flow path, the single element disadvantages such as determination efficiency is low one by one, it is difficult to meet the needs of contemporary industry rhythm of production.
Summary of the invention
It is an object of the invention to establish be used for and meanwhile measure in vanadium titanium blast furnace gas mud/ash content for 0.00001%~
The Specimen eliminating preparation method of your dilute constituent content such as 0.1% In, Sc, Ge, Ga, Sr, Zr, Co and elemental composition detection side
Method.To achieve the goals above, one aspect of the present invention provides the high temperature sintering and wet process acid of a kind of vanadium titanium blast furnace gas mud/ash
The molten sample solution resolution preparation method combined；On the other hand provide a kind of above-mentioned resolution preparation method be prepared it is molten
The detection method of your dilute constituent content in liquid.
First technical problem to be solved by this invention is to provide a kind of resolution vanadium titanium blast furnace gas mud/ash method.
Method includes the following steps:
Step A, calcination: by vanadium titanium blast furnace gas mud/ash in 550~650 DEG C of 30~40min of calcination, cooling；
Step B, it clears up:
1., in the cooling material of step A water, hydrofluoric acid and chloroazotic acid is added, be heated to solution boiling and cleared up；
2., be added dilute sulfuric acid, be heated to generating dense white cigarette mist；
3., concentrated nitric acid is added, be heated to generating dense white cigarette mist again and keep, it is cooling；
4., water and concentrated nitric acid is added, boil, cool down.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, the digestion time is 30
~40min.This digestion time refers to after water is added, hydrofluoric acid, chloroazotic acid are heated to solution boiling, under solution fluidized state after
The time of 30~40min of reaction is held in continuation of insurance.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, the quality of the hydrofluoric acid
Concentration is 40~47%.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, the chloroazotic acid is by concentrated hydrochloric acid
3 ﹕ 1 are mixed by volume with concentrated nitric acid.
Further, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, the matter of the concentrated hydrochloric acid
Measuring concentration is 36~38%.
Further, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, the matter of the concentrated nitric acid
Measuring concentration is 65~68%.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 10~15mL water.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 1.0~2.0mL hydrofluoric acid.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 1. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 15.0~20.0mL chloroazotic acid.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 2. in, the dilute sulfuric acid is dense sulphur
1 ﹕ 1 is mixed acid by volume with water.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 2. in, the quality of the concentrated sulfuric acid
Concentration is 95~98%.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 2. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 5.0~8.0mL dilute sulfuric acid.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 3. in, the quality of the concentrated nitric acid
Concentration is 65~68%.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 3. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 3.0~5.0mL concentrated nitric acid.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 3. in, it is described to remain holding 8
~15min.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 4. in, the quality of the concentrated nitric acid
Concentration is 65~68%.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 4. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 10~15mL water.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 4. in, every 0.5~1.0g vanadium titanium
Blast furnace gas mud/ash is corresponding to be added 10.0~15.0mL concentrated nitric acid.
Specifically, in the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, step B 4. in, it is described boil after keep 10
~15min.
Preferably, the method for above-mentioned resolution vanadium titanium blast furnace gas mud/ash, comprising the following steps: weigh vanadium titanium blast furnace gas
Mud/0.5~1.0g of ash is in 550~650 DEG C of 30~40min of calcination；After rinsing with 10~15mL water after cooling and disperse calcination
Sample, addition 1.0~2.0mL hydrofluoric acid, 15.0~20.0mL chloroazotic acid are heated to solution and boil, and continuation boiling reaction 30~
40min；Heating reaction to the dense white cigarette mist of sulfur trioxide that sulfuric acid decomposition generates is full of after 5.0~8.0mL (1+1) dilute sulfuric acid is added
Container；3.0~5.0mL concentrated nitric acid is added dropwise, continues 8~15min after heating reaction to the generation dense white cigarette mist of sulfur trioxide again, takes
Under be cooled to room temperature；With 10~15mL water flushing, be added 10.0~15.0mL nitric acid, heating boil 10~15min of solution to get
To digestion solution.
Second technical problem to be solved by this invention is to provide the method system of above-mentioned resolution vanadium titanium blast furnace gas mud/ash
Standby obtained digestion solution.
Third technical problem to be solved by this invention is to provide your dilute member in a kind of detection vanadium titanium blast furnace gas mud/ash
The method of cellulose content.Your dilute element includes In, Sc, Ge, Ga, Sr, Zr, Co.
The method for detecting your dilute constituent content in vanadium titanium blast furnace gas mud/ash, comprising the following steps:
A, the standard solution of the various concentration of metal to be measured is prepared with iron-based liquid solution, then uses inductively coupled plasma
Body atomic emission spectrometry (ICP-AES) detects standard solution, draws standard curve；
B, digestion solution is detected using inductively coupled plasma atomic emission spectrometry (ICP-AES), then
The concentration of metal to be measured is calculated by the standard curve that step A is obtained, obtains content.
Preferably, in above-mentioned detection method step A, the metal to be measured includes In, Sc, Ge, Ga, Sr, Zr or Co.
Preferably, in above-mentioned detection method step A, the condition of the inductively coupled plasma atomic emission spectrometry
Are as follows: radio-frequency power 1150W assists gas 1.0L/min, atomization gas pressure 0.23MPa, peristaltic pump pump speed 65r/min, observed altitude
12.0mm, time of integration 30s.
Preferably, in above-mentioned detection method step B, the condition of the inductively coupled plasma atomic emission spectrometry
Are as follows: radio-frequency power 1150W assists gas 1.0L/min, atomization gas pressure 0.23MPa, peristaltic pump pump speed 65r/min, observed altitude
12.0mm, time of integration 30s.
Preferably, in above-mentioned detection method step A, the condition of the inductively coupled plasma atomic emission spectrometry
Are as follows: element analysis spectrum line: element analysis spectrum line: In 230.606nm, Sc 361.384nm, Ge 204.171nm, Ga
294.364nm、Sr 407.771nm、Zr 339.198nm、Co 238.892nm。
Preferably, in above-mentioned detection method step B, the condition of the inductively coupled plasma atomic emission spectrometry
Are as follows: element analysis spectrum line: element analysis spectrum line: In 230.606nm, Sc 361.384nm, Ge 204.171nm, Ga
294.364nm、Sr 407.771nm、Zr 339.198nm、Co 238.892nm。
The method for detecting your dilute constituent content in vanadium titanium blast furnace gas mud/ash, comprising the following steps:
A, the standard solution for preparing the various concentration of metal to be measured, it is first using the Rh standard solution of 1~10ng/mL as internal standard
Then element detects standard solution using inductively coupled plasma mass spectrometry (ICP-MS), standard curve is drawn；
B, digestion solution is detected using inductively coupled plasma mass spectrometry, the mark then obtained by step A
The concentration of metal to be measured is calculated in directrix curve, obtains content.
Preferably, in above-mentioned detection method step A, the metal to be measured includes In, Sc, Ge, Ga, Sr, Zr or Co.
Preferably, in the above-mentioned detection method step A that disappears, the condition of the inductively coupled plasma mass spectrometry are as follows: radio frequency
Generator power 1150W, atomization gas flow velocity 0.75L/min, test solution lifting capacity 1.0mL/min, resolution ratio 0.7amu, measurement point/
Peak 21, scanning times 3, residence time 100ms.
Preferably, in the above-mentioned detection method step B that disappears, the condition of the inductively coupled plasma mass spectrometry are as follows: radio frequency
Generator power 1150W, atomization gas flow velocity 0.75L/min, test solution lifting capacity 1.0mL/min, resolution ratio 0.7amu, measurement point/
Peak 21, scanning times 3, residence time 100ms.
Preferably, in above-mentioned detection method step A, the condition of the inductively coupled plasma mass spectrometry are as follows: analysis is same
Position element and its abundance114.90In (95.10%),48.96Sc (100%),71.92Ge (27.54%),68.93Ga (60.11%),87.91Sr
(82.58%),89.90Zr (51.45%),58.93Co (100%).
Preferably, in above-mentioned detection method step B, the condition of the inductively coupled plasma mass spectrometry are as follows: analysis is same
Position element and its abundance114.90In (95.10%),48.96Sc (100%),71.92Ge (27.54%),68.93Ga (60.11%),87.91Sr
(82.58%),89.90Zr (51.45%),58.93Co (100%).
The method of the present invention using high temperature sintering with wet process acid is molten combine by the way of, and add according to designated order, opportunity
Enter particular agent and control wet chemistry reaction condition, it is ensured that In, Sc to be measured in vanadium titanium blast furnace gas mud/ash sample, Ge,
The Determination of Rare-Expensive Elements such as Ga, Sr, Zr, Co are reacted into sample solution by effective resolution, to ensure that the accurate of testing result
Property.
The method of the present invention application inductively coupled plasma body atomic emissions spectrum or inductivity coupled plasma mass spectrometry are as inspection
Survey means, the content of the Determination of Rare-Expensive Elements such as In, Sc, Ge, Ga, Sr, Zr, Co in sample solution prepared by Simultaneous Direct Determination,
Have the advantages that detection is accurate, Monitoring lower-cut is low etc..
Specific embodiment
Specimen eliminating solution manufacturing method of the present invention is the following steps are included: weigh vanadium titanium blast furnace gas mud/ash sample in porcelain
In boat, it is placed in calcination in high temperature furnace；Then, sample after calcination is transferred in polytetrafluoroethylene beaker, be added water, hydrofluoric acid and
Chloroazotic acid, heating carry out resolution reaction；Dilution heat of sulfuric acid is added, the reaction was continued to the generation dense white cigarette mist of sulfur trioxide；Dense nitre is added dropwise
Acid carries out Strong oxdiative reaction, and nitrogen oxides brown fume continues to be heated to generate the dense white cigarette mist number of sulfur trioxide once more after disappearing
Minute；Water is added after solution is cooling and nitric acid boils, cooling solution dilutes constant volume with water, to obtain detecting sample used molten
Liquid.
The present invention clears up vanadium titanium blast furnace gas mud/ash method, comprising the following steps:
A, calcination: weighing vanadium titanium blast furnace gas mud/0.5~1.0g of ash, in 550 DEG C~650 DEG C 30~40min of calcination；
B, it clears up:
1. rinsing and dispersing the sample after calcination after cooling with 10~15mL water, 1.0~2.0mL hydrofluoric acid, 15.0 is added
~20.0mL chloroazotic acid is heated to solution boiling, continues 30~40min of boiling reaction；
2. the dense white cigarette mist of sulfur trioxide that heating reaction is generated to sulfuric acid decomposition after 5.0~8.0mL (1+1) dilute sulfuric acid is added
Full of beaker；
3. be added dropwise 3.0~5.0mL concentrated nitric acid, continue heating reaction to again generate the dense white cigarette mist of sulfur trioxide after 8~
15min is removed and is cooled to room temperature；
4. 10.0~15.0mL nitric acid is added with the flushing of 10~15mL water, 10~15min of solution is boiled in heating；Solution is cold
But constant volume is diluted afterwards.
In the method for the present invention step A, if temperature is low, the time is short, calcination is insufficient, free carbon or carbide oxidation point
Solution not exclusively, influences the subsequent molten effect of acid；If temperature is high, the time is long, decomposition of components volatilization evolution loss to be measured is easily led to,
So control 30~40min of calcination at 550~650 DEG C of calcination temperature.
1. hydrofluoric acid, chloroazotic acid of the method for the present invention through step B sufficiently react a period of time with sample, most of easy in sample
Molten substance is resolved in pass into solution, and the step is mainly by generating ocratation form for matrix element pasc reaction in sample
Volatilization removes silica, to simplify sample solution matrix composition.
In the method for the present invention step B, through step, 1. hydrofluoric acid, chloroazotic acid sufficiently react a period of time with sample, in sample
After most of readily soluble substance is resolved in pass into solution, 2. sulfuric acid is just added in step, avoid in higher boiling sulfuric acid medium, low
Not yet substantially effectively just too early too fast evaporation escapes hydrofluoric acid, hydrochloric acid, the nitric acid of boiling point with example reaction.Sulfuric acid is added
Afterwards, a large amount of dense white cigarette mists of sulfur trioxide are generated by being heated at high temperature to decompose, promotes the Titanium base of indissoluble under this condition of high temperature
And your dilute element such as indium zirconium is sufficiently cleared up and is formed soluble sulphate and enters sample solution.
The method of the present invention step B 3. in, by the way that concentrated nitric acid is added under the condition of high temperature of sulfuric acid decomposition, in the concentrated sulfuric acid and
Further Strong oxdiative decomposes calcination remnants carbide in sample and indissoluble substance is promoted to disappear under the strong oxidizing property medium of concentrated nitric acid
Solution enters solution.After nitric acid Strong oxdiative is added, continues heating resolution reaction to generation sulphur trioxide mist again and kept for one section
Time further ensures that your dilute element to be measured is sufficiently effectively cleared up into solution in sample, while promoting in this small size
Under concentrated sulfuric acid medium, the lead element of high level in vanadium titanium blast furnace gas mud is formed into lead sulfate precipitation, simplifies sample solution base
Body composition.
The method of the present invention step B 4. in, be added water and nitric acid mainly for when dissolution sulfuric acid evaporation is smoldered because of solution body
Product reduces and the salt of precipitation.
In the method for the present invention step B, hydrofluoric acid is driven to the greatest extent by complete during sulfuric acid decomposition is smoldered twice, avoids its corrosion
The inlet system components such as quartz glass when subsequent detection in instrument and equipment, it is ensured that ICP-AES, ICP-MS detecting instrument can match
It sets using the portion with quartz glass materials such as higher nebulization efficiency, the better concentric atomizer of stability and swirling flow atomizing rooms
Part, it is ensured that detection method has the technical indicators such as better sensitivity, precision and Monitoring lower-cut.
The present invention measures the detection method of dilute scattered precious metal element ingredient in vanadium titanium blast furnace gas mud/ash, including following step
Rapid: ICP-AES is according to the progress Matrix Match correction of about 30% iron and synchronous background correction is contained in sample, using in iron-based liquid solution
It is middle that your dilute elemental standard solution to be measured is added, diluted with water prepare indium scandium germanium gallium strontium zirconium cobalt concentration be respectively 0.0,0.05,0.10,
1.0,5.0,10.0,7 of 50.0mg/L serial mixed standard solutions draw calibration curves；Digestion solution to be measured is measured, then
The concentration of metal to be measured is calculated by the standard curve that step A is obtained, obtains content.ICP-AES detection parameters: radio frequency function
Rate 1150W assists gas 1.0L/min, atomization gas pressure 0.23MPa, peristaltic pump pump speed 65r/min, observed altitude 12.0mm, product
30s between timesharing, element analysis spectrum line In 230.606nm, Sc 361.384nm, Ge 204.171nm, Ga 294.364nm, Sr
407.771nm、Zr 339.198nm、Co 238.892nm。
The present invention measures the detection method of dilute scattered precious metal element ingredient in vanadium titanium blast furnace gas mud/ash, including following step
It is rapid: ICP-MS take internal standard method correction of matrix effect influence, using the Rh standard solution of 1~10ng/mL as internal standard element, not into
Row Matrix Match directly dilutes elemental standard solution to be measured with water, prepare indium scandium germanium gallium strontium zirconium cobalt concentration be respectively 0.0,0.10,
0.50,7 serial mixed standard solutions drafting calibration curves of 1.0,5.0,10.0,50.0ng/mL；It is molten to measure resolution to be measured
Then the concentration of metal to be measured is calculated by the standard curve that step A is obtained, obtains content for liquid；If in sample solution to
The maximum concentration point that concentration of element is greater than calibration curve is surveyed, is divided after taking sample solution to be diluted in calibration curve concentration range with water
Measurement.ICP-MS detection parameters: radio-frequency signal generator power 1150W, atomization gas flow velocity 0.75L/min, test solution lifting capacity 1.0mL/
Min, resolution ratio 0.7amu, measurement point/peak 21, scanning times 3, residence time 100ms analyze isotope and its abundance114.90In
(95.10%),48.96Sc (100%),71.92Ge (27.54%),68.93Ga (60.11%),87.91Sr (82.58%),89.90Zr
(51.45%),58.93Co (100%).
Hereinafter, your dilute gold in the measurement vanadium titanium blast furnace gas mud (class) that the present invention will be described in detail will be carried out in conjunction with the embodiments
Belong to the resolution preparation method and its detection method of the sample solution of constituent content.
Come the method and effect of explanation and illustration the embodiment of the present invention below in conjunction with specific example.
In embodiments of the present invention, hydrofluoric acid is the most dense reagent of not diluted market sale, and mass percent is dense
Degree is 40~47%；Hydrochloric acid, nitric acid are also the most dense reagent of not diluted market sale, and mass percent concentration is respectively
36~38%, 65~68%；Chloroazotic acid is mixed by the concentrated hydrochloric acid and concentrated nitric acid of above-mentioned mass percent concentration according to 3 ﹕ of volume ratio, 1 relationship
It closes, i.e. 3 parts of concentrated hydrochloric acids are mixed with 1 part of concentrated nitric acid；Dilute sulfuric acid is the sulfuric acid solution of (1+1), according to volume ratio by 1 part
The concentrated sulfuric acid is slowly added to be uniformly mixed in 1 part of water while stirring and form, and wherein the concentrated sulfuric acid is not diluted market sale
Most dense reagent, mass percent concentration be 95~98%；Water be meet the distilled water of laboratory second level water requirement or go from
Sub- water；Equipment are as follows: match 6300 type inductively coupled plasma body atomic emissions spectrometer (ICP-AES) of Mo Feishier company and beauty in the U.S.
State's PE company ELAN9000 type icp ms (ICP-MS) but not limited to this.
Embodiment 1
The sample detection solution of vanadium titanium blast furnace gas mud clears up preparation
Vanadium titanium blast furnace gas mud sample (No. 1 sample) 0.50g is weighed in porcelain boat, is placed in high temperature furnace in 550 DEG C of calcinations
30min is transferred in polytetrafluoroethylene beaker after cooling, is rinsed wall of cup with 10mL water and is dispersed the sample after calcination, is added
1.0mL hydrofluoric acid, 15.0mL chloroazotic acid boil in heating reaction to solution on 300 DEG C~400 DEG C electric hot plates, continue resolution reaction
30min；5.0mL (1+1) dilute sulfuric acid is added, the dense white cigarette mist of a large amount of sulfur trioxides that heating reaction to sulfuric acid decomposition generates is full of burning
3.0mL concentrated nitric acid is added dropwise in cup；Continue heating to react to the generation dense white cigarette mist of sulfur trioxide again, and keep 8min, removes cooling
To room temperature；Wall of cup is rinsed with 10mL water, 10.0mL nitric acid is added, heating boils solution and keeps 10min；With water after solution is cooling
Dilute to volume in 50mL volumetric flask be uniformly mixed it is to be measured.
With the content of element in ICP-AES measurement sample detection solution
Measure the content of the elements such as In, Sc, Ge, Ga, Sr, Zr, Co in sample solution simultaneously using ICP-AES.According to sample
Carry out Matrix Match correction and synchronous background correction containing about 30% iron in product, using in iron-based liquid solution addition In, Sc, Ge,
The standard solution of Ga, Sr, Zr, Co, diluted with water prepare its concentration be respectively 0.0,0.05,0.10,1.0,5.0,10.0,
The serial mixed standard solution of 7 of 50.0mg/L, calibrates ICP-AES spectrometer with this and draws working curve；ICP-AES detection
Parameter: radio-frequency power 1150W assists gas 1.0L/min, atomization gas pressure 0.23MPa, peristaltic pump pump speed 65r/min, and observation is high
Spend 12.0mm, time of integration 30s, element analysis spectrum line In 230.606nm, Sc 361.384nm, Ge 204.171nm, Ga
294.364nm、Sr 407.771nm、Zr 339.198nm、Co 238.892nm。
Embodiment 2
Vanadium titanium blast furnace gas mud sample (No. 2 samples) 1.00g, 650 DEG C of calcination 40min are weighed, cooling is transferred in beaker
It is rinsed with 15mL water, dispersion sample, 2.0mL hydrofluoric acid is added, the heating reaction of 20.0mL chloroazotic acid is boiled and continued to solution
40min；8.0mL (1+1) dilute sulfuric acid is added, 5.0mL is added dropwise after being full of beaker to the dense white cigarette mist of a large amount of sulfur trioxides in heating reaction
Concentrated nitric acid；Continue heating again generate the dense white cigarette mist of sulfur trioxide after and keep 15min；Cooling is simultaneously rinsed with 15mL water, is added
15.0mL nitric acid boils solution and keeps 15min；After solution is cooling with water dilute to volume in 100mL volumetric flask be uniformly mixed to
It surveys.
In addition to this, the vanadium titanium blast furnace gas mud sample solution is prepared simultaneously according to method identical with the method for embodiment 1
With the content of elemental composition in ICP-AES measurement solution.
Embodiment 3
Vanadium titanium blast furnace dust sample (No. 3 samples) 0.80g, 600 DEG C of calcination 35min are weighed, cooling is transferred in beaker
With the flushing of 10mL water, 1.8mL hydrofluoric acid is added, 20.0mL chloroazotic acid is heated to solution and boils and continue 35min；7.0mL (1+ is added
1) dilute sulfuric acid is heated to generating the dense white cigarette mist of a large amount of sulfur trioxides, and 4.0mL concentrated nitric acid is added dropwise；The dense white cigarette of sulfur trioxide is generated again
15min is kept after mist；Cooling is simultaneously rinsed with 15mL water, and 10.0mL nitric acid is added, boils solution and keeps 13min；Solution is cooling
Afterwards with water dilute to volume in 100mL volumetric flask be uniformly mixed it is to be measured.
In addition to this, the vanadium titanium blast furnace gas mud sample solution is prepared simultaneously according to method identical with the method for embodiment 1
With the content of elemental composition in ICP-AES measurement solution.
Embodiment 4
The sample detection solution of vanadium titanium blast furnace dust clears up preparation
Vanadium titanium blast furnace dust sample (No. 4 samples) 0.50g, 600 DEG C of calcination 40min are weighed, cooling is transferred in beaker
With the flushing of 15mL water, 1.0mL hydrofluoric acid is added, 15.0mL chloroazotic acid is heated to solution and boils and continue 30min；5.0mL (1+ is added
1) dilute sulfuric acid is heated to generating the dense white cigarette mist of a large amount of sulfur trioxides, and 4.0mL concentrated nitric acid is added dropwise；The dense white cigarette of sulfur trioxide is generated again
10min is kept after mist；Cooling is simultaneously rinsed with 15mL water, and 10.0mL nitric acid is added, boils solution and keeps 10min；Solution is cooling
Afterwards with water dilute to volume in 100mL volumetric flask be uniformly mixed it is to be measured.
With the content of element in ICP-MS measurement sample detection solution
Measure the content of the elements such as In, Sc, Ge, Ga, Sr, Zr, Co in sample solution simultaneously using ICP-MS.With 5ng/mL
Rh standard solution as internal standard element, it is molten according to the proportionate relationship and sample of volume ratio 1:1 using online internal standard mixer
Mass spectrograph measurement is imported after liquid or calibration standard liquid mixing.Elemental standard solution to be measured is directly diluted with water, prepares indium scandium germanium gallium strontium
Zirconium cobalt concentration is respectively 7 serial mixed standard solutions of 0.0,0.10,0.50,1.0,5.0,10.0,50.0ng/mL, with this
Calibration ICP-MS spectrometer simultaneously draws calibration curve.ICP-MS detection parameters: radio-frequency signal generator power 1150W, atomization gas
Flow velocity 0.75L/min, test solution lifting capacity 1.0mL/min, resolution ratio 0.7amu, measurement point/peak 21, scanning times 3, residence time
100ms, analyze isotope and its abundance 114.90In (95.10%), 48.96Sc (100%), 71.92Ge (27.54%),
68.93Ga (60.11%), 87.91Sr (82.58%), 89.90Zr (51.45%), 58.93Co (100%).
Embodiment 5
Vanadium titanium blast furnace gas mud sample (No. 5 samples) 0.50g, 550 DEG C of calcination 35min are weighed, cooling is transferred in beaker
With the flushing of 10mL water, 1.5mL hydrofluoric acid is added, 20.0mL chloroazotic acid is heated to solution and boils and continue 35min；6.0mL (1+ is added
1) dilute sulfuric acid is heated to generating the dense white cigarette mist of a large amount of sulfur trioxides, and 5.0mL concentrated nitric acid is added dropwise；The dense white cigarette of sulfur trioxide is generated again
15min is kept after mist；Cooling is simultaneously rinsed with 10mL water, and 10.0mL nitric acid is added, boils solution and keeps 10min；Solution is cooling
Afterwards with water dilute to volume in 100mL volumetric flask be uniformly mixed it is to be measured.
In addition to this, the vanadium titanium blast furnace gas mud sample solution is prepared simultaneously according to method identical with the method for embodiment 4
With the content of elemental composition in ICP-MS measurement solution.
The assessment of 6 precision of embodiment
Repetition carries out 8 independent Specimen eliminating solution preparations and element to embodiment 1, embodiment 2 and embodiment 3 respectively
Assay, and statistics calculates the average value and relative standard deviation (RSD) of 8 measurement results respectively, to assess this method
Detection precision it is horizontal.It the results are shown in Table 1.
1 precision test of table (n=8)
Table 1 is surveyed as it can be seen that in ICP-AES method measurement vanadium titanium blast furnace gas mud (ash) sample when micro Determination of Rare-Expensive Elements
Determine relative standard deviation RSD < 5.0% of the above contents level of result 0.0x%, measurement result 0.0x%~0.00x% content water
Relative standard deviation RSD < 10.0% of flat range shows that multiplicating measurement result is consistent, and repeatability, the reproducibility of method are good
Good, method precision with higher is horizontal.
The assessment of 7 precision of embodiment
It repeats to carry out embodiment 4 and embodiment 5 respectively 8 independent Specimen eliminating solution preparations and constituent content is surveyed
It is fixed, and statistics calculates the average value and relative standard deviation (RSD) of 8 measurement results respectively, to assess the detection of this method
Precision is horizontal.It the results are shown in Table 2.
2 precision test of table (n=8)
Table 2 measures as it can be seen that in ICP-MS method measurement vanadium titanium blast furnace gas mud (ash) sample when micro Determination of Rare-Expensive Elements
As a result relative standard deviation RSD < 5.0% of 0.00x% contents level, measurement result 0.00x%~0.000x% contents level
Relative standard deviation RSD < 10.0%, show be repeated several times measurement result it is consistent, repeatability, the reproducibility of method are good, side
Method precision with higher is horizontal.
8 Accuracy evaluation of embodiment
The present invention carries out mark-on reclaims test to No. 1 sample and No. 3 samples.It is measured first by embodiment 1 and embodiment 3
The original amount of contained In, Sc, Ge, Ga, Sr, Zr, Co in No. 1 sample and No. 3 samples；Then respectively No. 1 sample, 3
The standard solution of the element to be measured of respective concentration is added in number sample, whole process repeats the sample of embodiment 1 and embodiment 3 respectively
Preparation and detection operation, by the assessment of the rate of recovery to verify sample solution preparation method and detection method of the invention.Examination
It tests and the results are shown in Table 3.
3 recovery test of table
Table 3 as it can be seen that the rate of recovery be 86%~114%, show analyze result accuracy and reliability with higher.
9 Accuracy evaluation of embodiment
The present invention carries out mark-on reclaims test to No. 4 samples and No. 5 samples.It is measured first by embodiment 4 and embodiment 5
The original amount of contained In, Sc, Ge, Ga, Sr, Zr, Co in No. 4 samples and No. 5 samples；Then respectively No. 4 samples, 5
The standard solution of the element to be measured of respective concentration is added in number sample, whole process repeats the sample of embodiment 4 and embodiment 5 respectively
Preparation and detection operation, by the assessment of the rate of recovery to verify sample solution preparation method and detection method of the invention.Examination
It tests and the results are shown in Table 4.
4 recovery test of table
Table 4 as it can be seen that the rate of recovery be 84%~116%, show analyze result accuracy and reliability with higher.
Although having been combined exemplary embodiment has shown and described the present invention, but the invention is not restricted to this.It is not taking off
In the case where from spirit or teaching of the invention, modification and variation can be made to embodiment.
Claims (9)
1. clearing up vanadium titanium blast furnace gas mud/ash method, it is characterised in that: the following steps are included:
Step A, calcination: by vanadium titanium blast furnace gas mud/ash in 550~650 DEG C of 30~40min of calcination, cooling；
Step B, it clears up:
1., in the cooling material of step A water, hydrofluoric acid and chloroazotic acid is added, be heated to solution boiling and cleared up；
2., be added dilute sulfuric acid, be heated to generating dense white cigarette mist；
3., concentrated nitric acid is added, be heated to generating dense white cigarette mist again and keep, it is cooling；
4., water and concentrated nitric acid is added, boil, cool down.
2. in resolution vanadium titanium blast furnace gas mud/ash method according to claim 1, it is characterised in that: step B is 1.
In, at least meet following any one:
The digestion time is 30~40min；
The mass concentration of the hydrofluoric acid is 40~47%；
By concentrated hydrochloric acid and concentrated nitric acid, 3 ﹕ 1 are mixed the chloroazotic acid by volume；
The mass concentration of the concentrated hydrochloric acid is 36~38%；
The mass concentration of the concentrated nitric acid is 65~68%；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 10~15mL water；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 1.0~2.0mL hydrofluoric acid；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 15.0~20.0mL chloroazotic acid.
3. in resolution vanadium titanium blast furnace gas mud/ash method according to claim 1 or 2, it is characterised in that: step B's
In 2., at least meet following any one:
The dilute sulfuric acid is that 1 ﹕ 1 is mixed by volume for the concentrated sulfuric acid and water；
The mass concentration of the concentrated sulfuric acid is 95~98%；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 5.0~8.0mL dilute sulfuric acid.
4. according to claim 1~3 in described in any item resolution vanadium titanium blast furnace gas mud/ash methods, it is characterised in that: step
Rapid B 3. in, at least meet following any one:
The mass concentration of the concentrated nitric acid is 65~68%；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 3.0~5.0mL concentrated nitric acid；
It is described to remain 8~15min of holding.
5. in resolution vanadium titanium blast furnace gas mud/ash method according to any one of claims 1 to 4, it is characterised in that: step
Rapid B 4. in, at least meet following any one:
The mass concentration of the concentrated nitric acid is 65~68%；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 10~15mL water；
Every 0.5~1.0g vanadium titanium blast furnace gas mud/ash is corresponding to be added 10.0~15.0mL concentrated nitric acid；
It is described to boil 10~15min.
6. according to claim 1~5 in described in any item resolution vanadium titanium blast furnace gas mud/ash methods, it is characterised in that: packet
It includes following steps: weighing vanadium titanium blast furnace gas mud/0.5~1.0g of ash in 550~650 DEG C of 30~40min of calcination；With 10 after cooling
~15mL water rinses and disperses the sample after calcination, and addition 1.0~2.0mL hydrofluoric acid, 15.0~20.0mL chloroazotic acid are heated to molten
Liquid boiling, continues 30~40min of boiling reaction；Heating reaction to sulfuric acid decomposition produces after 5.0~8.0mL (1+1) dilute sulfuric acid is added
The dense white cigarette mist of raw sulfur trioxide is full of container；3.0~5.0mL concentrated nitric acid is added dropwise, continues heating reaction to generating three oxygen again
8~15min after the change dense white cigarette mist of sulphur, removes and is cooled to room temperature；With the flushing of 10~15mL water, 10.0~15.0mL nitric acid is added,
Heating boils 10~15min of solution to get digestion solution is arrived.
7. the digestion solution being prepared by any one of claim 1~6 resolution vanadium titanium blast furnace gas mud/ash method.
8. the method for detecting your dilute constituent content in vanadium titanium blast furnace gas mud/ash, it is characterised in that: the following steps are included:
A, the standard solution of the various concentration of metal to be measured is prepared with iron-based liquid solution, it is then former using inductively coupled plasma body
Sub- emission spectrometry detects standard solution, draws standard curve；
B, digestion solution as claimed in claim 7 is detected using inductively coupled plasma atomic emission spectrometry, so
The concentration of metal to be measured is calculated by the standard curve that step A is obtained afterwards, obtains content；
Preferably, in step A or B, the condition of the inductively coupled plasma atomic emission spectrometry are as follows: radio-frequency power
1150W assists gas 1.0L/min, atomization gas pressure 0.23MPa, peristaltic pump pump speed 65r/min, observed altitude 12.0mm, integral
Time 30s；
Preferably, in step A or B, the condition of the inductively coupled plasma atomic emission spectrometry are as follows: elemental analysis spectrum
Line: element analysis spectrum line: In 230.606nm, Sc 361.384nm, Ge 204.171nm, Ga 294.364nm, Sr
407.771nm、Zr 339.198nm、Co 238.892nm。
9. the method for detecting your dilute constituent content in vanadium titanium blast furnace gas mud/ash, it is characterised in that: the following steps are included:
A, the standard solution for preparing the various concentration of metal to be measured, using the Rh standard solution of 1~10ng/mL as internal standard element,
Then standard solution is detected using inductively coupled plasma mass spectrometry, draws standard curve；
B, digestion solution as claimed in claim 7 is detected using inductively coupled plasma mass spectrometry, then passes through step
The concentration of metal to be measured is calculated in the standard curve that rapid A is obtained, and obtains content；
Preferably, in step A or B, the condition of the inductively coupled plasma mass spectrometry are as follows: radio-frequency signal generator power 1150W,
Atomization gas flow velocity 0.75L/min, test solution lifting capacity 1.0mL/min, resolution ratio 0.7amu, measurement point/peak 21, scanning times 3 are stayed
Stay time 100ms；
Preferably, in step A or B, the condition of the inductively coupled plasma mass spectrometry are as follows: analysis isotope and its rich
Degree114.90In (95.10%),48.96Sc (100%),71.92Ge (27.54%),68.93Ga (60.11%),87.91Sr (82.58%)
、89.90Zr (51.45%),58.93Co (100%).
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