CN109580326A - The measuring method of zinc oxide and alkali metal in a kind of dedusting ash - Google Patents
The measuring method of zinc oxide and alkali metal in a kind of dedusting ash Download PDFInfo
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- CN109580326A CN109580326A CN201811479891.8A CN201811479891A CN109580326A CN 109580326 A CN109580326 A CN 109580326A CN 201811479891 A CN201811479891 A CN 201811479891A CN 109580326 A CN109580326 A CN 109580326A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
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- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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Abstract
The present invention relates to metal detection technical fields, more particularly in a kind of dedusting ash zinc oxide and alkali metal measuring method, it is measured using x ray fluorescence spectrometry, sample is handled using fusion method, → igloss pre-oxidizes → produces sample → sample detection → interpretation of result specifically includes the following steps: sample pretreatment.The present invention can be achieved to carry out the content of zinc oxide and alkali metal in all kinds of dedusting ash fast and accurately analysis measurement, it is measured using content of the fusion method to zinc oxide in dedusting ash and alkali metal, granularity effect, the mineral effect that sample can be eliminated, do not damage analyzer.
Description
Technical field
The present invention relates to the measurement sides of zinc oxide and alkali metal in metal detection technical field more particularly to a kind of dedusting ash
Method.
Background technique
The processes such as sintering, blast furnace, converter, electric furnace can produce a large amount of dust and its byproduct, be referred to as dedusting ash, remove
The general 200 mesh sieving rate of the fineness of dust is in 50--65%, even more carefully, easily drifts in an atmosphere, if not being subject to effective benefit
With, ambient enviroment is seriously polluted, and the zinc and alkali metal that contain in dedusting ash can adversely affect operation of blast furnace.Wherein,
Zinc oxide can be enriched in blast fumance system circulation, to the life of the blast furnace, high and stable yields, iron ore and coke property, blast furnace operating
And have an adverse effect to blast furnace heat distribution etc..Alkali metal (K20、Na20) metallurgical performance of coke can be deteriorated, make coke ratio liter
Height destroys furnace condition anterograde, corrodes furnace wall, reduces the life of the blast furnace.
If reasonably developed and used to dedusting ash, secondary pollution can be not only prevented, and can also turn waste into wealth, made
It is utilized for secondary resource, walks the Road of Cyclic Economy, build gueen factory.In the prior art, to the Land use systems master of dedusting ash
Have: pellet is made and recycles and as raw material for purifying non-ferrous metal etc..No matter however which kind of Land use systems, remove
The content of zinc oxide and alkali metal is all to be related to the important indicator of dedusting ash price and technology controlling and process in dust, therefore to all kinds of
The content of zinc oxide and alkali metal carries out fast and accurately analysis measurement in dedusting ash, not only for the scientific classification of dedusting ash
And comprehensive utilization provides data and supports, can also have important to sintering and blast furnace production process process improving and stable operation
Reference significance.
Summary of the invention
To solve the above problems, the invention discloses the measuring methods of zinc oxide and alkali metal in a kind of dedusting ash, specifically
Technical solution is as follows:
The measuring method of zinc oxide and alkali metal in a kind of dedusting ash, is measured using x ray fluorescence spectrometry, is utilized
Fusion method handles sample, specifically includes the following steps: sample pretreatment → igloss pre-oxidizes → produce the detection of sample → sample →
Interpretation of result.
Preferably, dedusting ash sample is first put into 105 DEG C ± 5 DEG C of air dry oven in the sample pretreatment step
It is middle to dry 1~2 hour, it is dried to constant weight.
Preferably, sample is gradually warming up to 230 in high temperature furnace since room temperature in the igloss pre-oxidation step
DEG C, heating rate is 10 DEG C/min, then keeps the temperature 30 minutes under the conditions of 230 DEG C, and then according to sample type difference, selection is not
Same temperature carries out calcination, then takes out, is put in drier and is cooled to room temperature, and weighs rapidly, sample burning decrement is as the following formula
It calculates:
M1: the quality of sample and cupel, g after calcination
M0: cupel quality, g
M: the quality of sample, g before calcination.
Preferably, bag-type dust ash sample, calcination temperature is 490 DEG C~510 DEG C, calcination 1.5~2.5 hours.
Preferably, mine slot dedusting ash and converter dust-removing ash sample, burning temperature is 800~950 DEG C, calcination 1~5 hour.
Preferably, the sample of producing method particularly includes: successively weigh dedusting ash sample, cobalt sesquioxide, mixing
Then bromination lithium reagent is added in platinum crucible in flux, the platinum crucible for filling sample is put into molten model machine and carries out molten sample,
It is spare that sample is taken out after the completion of molten model machine melts sample, after being cooled to room temperature；The mixed solvent is the tetraboric acid of mass fraction 67%
The mixed solvent that the lithium metaborate of lithium and mass fraction 33% forms.
Preferably, the sample of producing method particularly includes: dedusting ash sample after successively weighing pre-oxidation treatment
0.3000g, cobalt sesquioxide 0.1000g, mixed flux 7.0000g are added bromination lithium reagent, will fill examination in platinum crucible
The platinum crucible of sample, which is put into molten model machine, carries out molten sample, and after the completion of melting the molten sample of model machine, it is spare that sample is taken out after being cooled to room temperature；Three
It is pure to analyze to aoxidize two cobalts, and the concentration of bromination lithium reagent is 50g/100ml.
Preferably, the sample detection uses Panaco X- Fluorescence Spectrometer AXiosMAX PW4400, using the end 4KW
The super sharp ceramic X-ray tube of window rhodium target.
The preparation of standard sample: selecting existing standard sample, and according to sample content, uses zinc oxide and sodium carbonate base
Quasi- substance prepares inner quality standard sample, after calcination, is reduced conversion content according to burning.Following standard sample is selected, according to above-mentioned system
Coupons are made in the method melting materialsed.Content of the corresponding test elements in standard sample is as shown in table 1 below.
Content of 1. test elements of table in standard sample
Panaco X- Fluorescence Spectrometer AXiosMAX is opened, Na, K, Zn spectral intensity in sequentially determining print use
SuperQ Software on Drawing spectral intensity-mass fraction working curve.
Correcting mode are as follows: Ci=LOi+Di+Ei*Ri*[1+Mi] C is concentration, LO is overlap of spectral lines correction, intercept D, slope E,
1+MiAbsorption enhancement effect between element, R are intensity.
The spectral intensity for measuring potassium sodium zinc in print, from the quality point for obtaining potassium sodium zinc in sample to be tested in working curve
Number.Beneficial effects of the present invention
Dedusting ash is different from the product of quantitative control production, is the byproduct under a kind of high temperature, and ingredient mutually fluctuates greatly with object,
The present invention has grasped difference by the condition test to sample by carrying out detailed analysis to different types of dedusting ash component
At a temperature of sample various physicochemical change situations, establish working curve, realize the analysis of fusion method x ray fluorescence spectrometry
The content of zinc and alkali metal in dedusting ash.
The present invention is measured the content of zinc oxide in dedusting ash and alkali metal using fusion method, can eliminate sample
Granularity effect, mineral effect are not damaged analyzer, are precisely controlled to sample disposition, except carbon, oxidation metal therein at
Divide (mainly fe) and sulphur etc., to prevent from damaging platinum crucible in sample melting process, while preventing to low-temperature metal
Scaling loss.
The present invention can accurately detect sintering machine head end dedusting ash, the iron-content of sintering machine tail dedusting ash, zinc oxide content and oxygen
Change the content of potassium；Accurate detection furnace cloth bag dust-removing ash, blast furnace gravitational dust collection ash, the iron-content of blast furnace ore tank dedusting ash, oxidation
Zinc and alkali metal content；Iron-content, zinc oxide and the alkali metal content of accurate detection dedusting steel-smelting converter ash, electric stove dust ash,
And other position dedusting ash iron-content, zinc oxide and alkali metal contents.
The present invention realize seven kinds or more cover sintering, ironmaking, steel making working procedure dedusting ash in zinc and alkali metal detection
Sintered material dedusting ash, sinter machine discharge end dedusting ash, screening dedusting ash and blast furnace environmental dust removal ash etc. are examined in normalization in time,
Corresponding data is provided.Gravitational dust collection ash has been no longer participate in sintered material after detection starts, and it is suitable to blast furnace to reduce harmful element
Capable adverse effect.Take-away for sintering machine head end dedusting ash, ironmaking bag-type dust ash etc. provides detection data, and realizes to richness
Collection oxidation Direct spectrophotometry.
Specific embodiment:
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but this
Invention is not limited thereto.
Embodiment 1
The measuring method of zinc oxide and alkali metal in bag-type dust ash, comprising the following steps:
1. sample pretreatment: mixing material, the sample of dedusting ash need to first be put into 105 DEG C ± 5 DEG C of air dry oven and dry 1.5
Hour or so, it is dried to constant weight.
2. igloss pre-oxidizes: due to the C simple substance (C >=0.5%) and other metallic iron lists in dedusting ash containing different content
Matter needs to carry out igloss pre-oxidation step.
2.1, which weigh sample after about 1.000g is dried (2-3, as a result report average value), is placed in the cupel of preparatory constant weight, essence
Really to 0.0002g.
Load weighted sample is placed on nickel crucible frame and is carefully placed into Muffle furnace by 2.2, and sample gradually rises since room temperature
Height, and kept for a period of time at 230 DEG C and suitably open the fire door of high temperature furnace, 500 DEG C are then warming up to, calcination 1.5 hours, is removed
The oxidants such as lithium nitrate are added in carbon, oxidized metal iron when necessary；It then takes out and (prevents skin ambustion, band puts high temperature gloves) and put
It is cooled to room temperature in drier, weighs rapidly.
The calculating of burning decrement in 2.3 samples:
M1: the quality of sample and cupel, g after calcination
M0: cupel quality, g
M: the quality of sample, g
3. producing sample:
Sample 0.3000g (being accurate to 0.0001g) is weighed in order, cobalt oxide 0.1000g (being accurate to 0.0001g), is mixed
Flux 7.0000g (being accurate to 0.0001g) is closed in platinum crucible, bromination lithium reagent (50g/100ml) 10 is added by regulation and drips.
The platinum crucible for filling sample is put into molten model machine, automatic running button is pressed, model machine is melted and enters molten sample state.It is molten
After the completion of model machine melts sample, takes out platinum crucible and be placed on ceramic wafer cooling, sample cooling after a week along a direction jog
To room temperature, bushing terminal is clamped with tweezers and is buckled to cooling on asbestos gauge, and observe sample whether there is or not obvious crackle and bubble, if any
Bubble, crackle or slag-off phenomenon should claim sample to melt again.
4. sample detects:
The print of passed examination is put into sample cup, the SuperQ Manager software of fluorescence detector is opened, is clicked
Measure and Analyse button inputs user name and password, opens measurement sample list and enters Sample Changer circle
Face.Add Measurement is clicked, then Routine is selected in Type drop-down menu again, in Application drop-down menu
Middle selection chuchenhui working curve, and input sample is numbered in Sample identification, then clicks Add
Sample is added in measurement list.
Over view is clicked, measure is clicked, starts to measure.
The specific measuring condition of the X- Fluorescence Spectrometer is as shown in table 2 below:
2. measuring condition of table
5. interpretation of result
After being measured, the Results Evaluation clicked in the interface SuperQ Manager (is selected to be shown
As a result) program checks result.X-fluorescence is shown that detected value input igloss numerical value recalculate you can get it corresponding detection
As a result.Testing result is as shown in table 3.
3. testing result of table
As can be seen from Table 2, the stability of this method, repeatability and accuracy are all preferable, meet sintering, ironmaking, refining
The requirement of the detection of zinc and alkali metal in the dedusting ash of steel process.
Embodiment 2
The measuring method of zinc oxide and alkali metal in mine slot dedusting ash, comprising the following steps:
1. sample pretreatment: it is small that mixing is expected, the sample of dedusting ash need to first be put into baking 1 in 105 DEG C ± 5 DEG C of air dry oven
When or so, it is dried to constant weight.
2. igloss pre-oxidizes: due to the C simple substance (C >=0.5%) and other metallic iron lists in dedusting ash containing different content
Matter needs to carry out igloss pre-oxidation step.
2.1, which weigh sample after about 1.000g is dried (2-3, as a result report average value), is placed in the cupel of preparatory constant weight, essence
Really to 0.0002g.
Load weighted sample is placed on nickel crucible frame and is carefully placed into Muffle furnace by 2.2, and sample gradually rises since room temperature
Height, heating rate is 10 DEG C/min, and is kept for 30 minutes at 230 DEG C, and suitably opens the fire door of high temperature furnace, is then warming up to
950 DEG C calcination 1 hour or more, then take out and (prevent skin ambustion, band puts high temperature gloves) to be put in drier and be cooled to room temperature,
It weighs rapidly.
The calculating of burning decrement in 2.3 samples:
M1: the quality of sample and cupel, g after calcination
M0: cupel quality, g
M: the quality of sample, g
3. producing sample:
Sample 0.3000g (being accurate to 0.0001g) is weighed in order, cobalt sesquioxide 0.1000g (is accurate to
0.0001g), bromination lithium reagent (50g/ is added by regulation in platinum crucible in mixed flux 7.0000g (being accurate to 0.0001g)
100ml) 10 drop.
The platinum crucible for filling sample is put into molten model machine, automatic running button is pressed, model machine is melted and enters molten sample state.It is molten
After the completion of model machine melts sample, takes out platinum crucible and be placed on ceramic wafer cooling, sample cooling after a week along a direction jog
To room temperature, bushing terminal is clamped with tweezers and is buckled to cooling on asbestos gauge, and observe sample whether there is or not obvious crackle and bubble, if any
Bubble, crackle or slag-off phenomenon should claim sample to melt again.
4. sample detects:
The print of passed examination is put into sample cup, the SuperQ Manager software of fluorescence detector is opened, is clicked
Measure and Analyse button inputs user name and password, opens measurement sample list and enters Sample Changer circle
Face.Add Measurement is clicked, then Routine is selected in Type drop-down menu again, in Application drop-down menu
Middle selection chuchenhui working curve, and input sample is numbered in Sample identification, then clicks Add
Sample is added in measurement list.
Over view is clicked, measure is clicked, starts to measure.
5. interpretation of result
After being measured, the Results Evaluation clicked in the interface SuperQ Manager (is selected to be shown
As a result) program checks result.X-fluorescence is shown that detected value input igloss numerical value recalculate you can get it corresponding detection
As a result.
Embodiment 3
The measuring method of zinc oxide and alkali metal in converter dust-removing ash, comprising the following steps:
1. sample pretreatment: it is small that mixing is expected, the sample of dedusting ash need to first be put into baking 2 in 105 DEG C ± 5 DEG C of air dry oven
When or so, it is dried to constant weight.
2. igloss pre-oxidizes: due to the C simple substance (C >=0.5%) and other metallic iron lists in dedusting ash containing different content
Matter needs to carry out igloss pre-oxidation step.
2.1, which weigh sample after about 1.000g is dried (2-3, as a result report average value), is placed in the cupel of preparatory constant weight, essence
Really to 0.0002g.
Load weighted sample is placed on nickel crucible frame and is carefully placed into Muffle furnace by 2.2, and sample gradually rises since room temperature
Height, heating rate is 10 DEG C/min, and is kept for 30 minutes at 230 DEG C, and suitably opens the fire door of high temperature furnace, is then warming up to
800 DEG C calcination 5 hours, then take out and (prevent skin ambustion, band puts high temperature gloves) to be put in drier and be cooled to room temperature, rapidly
It weighs.
The calculating of burning decrement in 2.3 samples:
M1: the quality of sample and cupel, g after calcination
M0: cupel quality, g
M: the quality of sample, g
3. producing sample:
Sample 0.3000g (being accurate to 0.0001g) is weighed in order, cobalt sesquioxide 0.1000g (is accurate to
0.0001g), bromination lithium reagent (50g/ is added by regulation in platinum crucible in mixed flux 7.0000g (being accurate to 0.0001g)
100ml) 10 drop.
The platinum crucible for filling sample is put into molten model machine, automatic running button is pressed, model machine is melted and enters molten sample state.It is molten
After the completion of model machine melts sample, takes out platinum crucible and be placed on ceramic wafer cooling, sample cooling after a week along a direction jog
To room temperature, bushing terminal is clamped with tweezers and is buckled to cooling on asbestos gauge, and observe sample whether there is or not obvious crackle and bubble, if any
Bubble, crackle or slag-off phenomenon should claim sample to melt again.
4. sample detects:
The print of passed examination is put into sample cup, the SuperQ Manager software of fluorescence detector is opened, is clicked
Measure and Analyse button inputs user name and password, opens measurement sample list and enters Sample Changer circle
Face.Add Measurement is clicked, then Routine is selected in Type drop-down menu again, in Application drop-down menu
Middle selection chuchenhui working curve, and input sample is numbered in Sample identification, then clicks Add
Sample is added in measurement list.
Over view is clicked, measure is clicked, starts to measure.
5. interpretation of result
After being measured, the Results Evaluation clicked in the interface SuperQ Manager (is selected to be shown
As a result) program checks result.X-fluorescence is shown that detected value input igloss numerical value recalculate you can get it corresponding detection
As a result.
Claims (9)
1. the measuring method of zinc oxide and alkali metal in a kind of dedusting ash, which is characterized in that carried out using x ray fluorescence spectrometry
Measurement handles sample using fusion method, specifically includes the following steps: sample pretreatment, → igloss pre-oxidizes → produces sample → examination
Sample detection → interpretation of result.
2. measuring method according to claim 1, which is characterized in that in the sample pretreatment step, dedusting ash sample
It is first put into 105 DEG C ± 5 DEG C of air dry oven and dries 1~2 hour, dried to constant weight.
3. measuring method according to claim 1, which is characterized in that in the igloss pre-oxidation step, sample is in high temperature
230 DEG C are gradually warming up in furnace since room temperature, heating rate is 10 DEG C/min, 30 minutes then are kept the temperature under the conditions of 230 DEG C,
Then it according to sample type difference, selects different temperature to carry out calcination, then takes out, be put in drier and be cooled to room temperature,
It weighs rapidly, sample burning decrement is calculated as follows:
M1: the quality of sample and cupel, g after calcination
M0: cupel quality, g
M: the quality of sample, g before calcination.
4. measuring method according to claim 3, which is characterized in that bag-type dust ash sample, calcination temperature be 490 DEG C~
510 DEG C, calcination 1.5~2.5 hours.
5. measuring method according to claim 3, which is characterized in that mine slot dedusting ash and converter dust-removing ash sample, calcination
Temperature is 800~950 DEG C, calcination 1~5 hour.
6. measuring method according to claim 1, which is characterized in that the sample of producing method particularly includes: successively claim
Dust sample, cobalt sesquioxide, mixed flux are removed in platinum crucible, bromination lithium reagent is then added, sample will be filled
Platinum crucible, which is put into molten model machine, carries out molten sample, and after the completion of melting the molten sample of model machine, it is spare that sample is taken out after being cooled to room temperature；It is described mixed
Bonding solvent is the mixed solvent that the lithium tetraborate of mass fraction 67% and the lithium metaborate of mass fraction 33% form.
7. measuring method according to claim 6, which is characterized in that the sample of producing method particularly includes: successively claim
Dedusting ash sample 0.3000g, cobalt sesquioxide 0.1000g, mixed flux 7.0000g after taking pre-oxidation treatment is in platinum crucible
In, bromination lithium reagent is added, the platinum crucible for filling sample is put into molten model machine and carries out molten sample, after the completion of melting the molten sample of model machine,
It is spare that sample is taken out after being cooled to room temperature；Cobalt sesquioxide is that analysis is pure, and the concentration of bromination lithium reagent is 50g/100ml.
8. measuring method according to claim 1, which is characterized in that the sample detection uses X- Fluorescence Spectrometer, adopts
With the super sharp ceramic X-ray tube of 4KW end window rhodium target, X- Fluorescence Spectrometer is opened, Na, K, Zn spectral intensity in sequentially determining print,
Spectral intensity-mass fraction working curve is drawn, the specific measuring condition of the X- Fluorescence Spectrometer is as shown in the table:
。
9. measuring method according to claim 8, which is characterized in that according to sample content, use zinc oxide and sodium carbonate
Primary standard substance prepares inner quality standard sample, after calcination, is reduced conversion content according to burning, corresponding test elements are in standard sample
Content it is as shown in the table:
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Application publication date: 20190405 |