CN110118792A - A kind of pressed powder method for making sample of ferroalloy productor and raw material - Google Patents
A kind of pressed powder method for making sample of ferroalloy productor and raw material Download PDFInfo
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- CN110118792A CN110118792A CN201810121492.8A CN201810121492A CN110118792A CN 110118792 A CN110118792 A CN 110118792A CN 201810121492 A CN201810121492 A CN 201810121492A CN 110118792 A CN110118792 A CN 110118792A
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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
- 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
Abstract
The pressed powder method for making sample of of the invention a kind of ferroalloy productor and raw material, specifically by step (1) sample for chemical analysis processed and drying, step (2) spectrum press sheet compression processed, the round print of step (3) pressure standard specification, the method, current chemical analysis method is substituted completely, the chemical component that primary and secondary quantitative elements or compound in ferroalloy productor and raw material are directly analyzed with energy dispersion type Xray fluorescence spectrometer achieves satisfactory analysis result, with certain novelty, it no matter theoretically or is experimentally all theoretical to pressed powder in Xray fluorescence spectrometer analysis and application abundant and development, with certain theory significance and practical value.
Description
Technical field
The invention belongs to prepare test sample, specifically a kind of Xray fluorescence spectrometer analysis iron that is suitable for is closed
The pressed powder method for making sample of golden product and raw material.
Background technique
Ferroalloy, which refers to be added in molten iron when steel-making as deoxidier, element additive etc., makes steel have certain characteristic or reach
A kind of product required to certain.China is the production of qualified the first in the world big ferroalloy, consumption and big export country, at present
Usage amount it is big be silicon systems, manganese systems, the big ferroalloy productor of chromium system three.For ferroalloy manufacturing enterprise, stokehold product classification storage
And batching factory, it requires to carry out chemical analysis measurement to chemical component.And the purchased raw material of ferroalloy smelting (silica, chromite,
Manganese ore, iron charge etc.) chemical constituents determination is also carried out, analysis data are for instructing smelting process production operation and contract knot
It calculates.Now the overwhelming majority detection method that uses of enterprises with the capacity analysis of wet bench, gravimetric analysis, spectrophotometric analysis,
Based on the analysis of Atomic absorption luminosity, using traditional wet chemistry analytic approach, needs to measure coherent element content one by one, operate numerous
Trivial, step is tediously long, need to put into more manpower, analyzes the slow low efficiency of speed, and analyze result accuracy and stability often
It is affected because of operator's experience and level, in addition needs to be used in combination strong acid, highly basic and other in analytic process
Chemical reagent, testing cost is high, be easy to cause personal injury or environmental pollution.Iron is closed using traditional wet chemistry analytic approach
Determination of trace elements in golden product and raw material, the level for being limited to analysis condition and laboratory personnel are generally more difficult.
It is continuous with large-scale analysis of modernization instrument and equipment Xray fluorescence spectrometer analytical technology and its computer software
Exploitation, so that the function of energy dispersion type Xray fluorescence spectrometer is gradually perfect.It can not only measure simultaneously nearly all in sample
Element, and have sample preparation is simple, analysis speed is fast, accuracy is high, favorable reproducibility, to sample without damage, free from environmental pollution
And the advantages that low consumption, the numerous areas such as geology, metallurgy, chemical industry, material, petroleum, medical treatment, archaeology are widely used in, it is especially domestic
Energy-dispersion X-ray fluorescence spectrometer is cheap, afford general enterprise can, can also afford to use, to realize use
One instrument can achieve the purpose that control full factory's quality.Therefore energy-dispersion X-ray fluorescence spectrometer has become one kind
Strong qualitative and accurate quantification analysis and testing technology, the increasingly attention by analysis worker and manufacturing enterprise.By
Be not suitable for directly analyzing in the physical state of ferroalloy productor and raw material, it is necessary to handle its sample, prepare suitable X and penetrate
The sample of line spectrofluorimetry, and sample preparation directly affects the speed of measurement and the accuracy of measurement result.It is glimmering in X-ray
In light spectrum analysis, there are mainly three types of methods for the sample preparation of ferroalloy field: powder pressing method, fusion method and centrifugal casting.
Fusion method can eliminate matrix effect and grain effect, to make the accuracy for analyzing result and precision greatly improve, still
Sample preparation is complicated for operation, the period is long, more demanding to operative skill.Not applicable ferroalloy enterprise analyzes batch samples,
And elemental metals when pre-oxidizing in ferroalloy do not aoxidize certain corrosivity to Pt-Au crucible completely, influences Pt-Au
Crucible continues to use.Centrifugal casting can also eliminate matrix effect and grain effect, though not corroding the danger of crucible, need
To use expensive high-frequency melting equipment, and be melted under applying argon gas protective condition after evacuation, through centrifugal casting to graphite or
Reguline metal sample is made in copper mold, to meet X-ray fluorescence spectra analysis, analysis cost is high, analyzes speed and chemical method
Do not significantly improve.Powder pressing method is a kind of ideal environmentally protective method for making sample, has the advantages that simple, quick, economy,
But have a important prerequisite, seek to grind in sample it is finely ground very uniformly, so that the measurement intensity of X-ray is reached constant, in this way
It could eliminate and reduce the influence of granularity and mineral effect.We are actually using existing some pressed powder method for making sample
It finds in the process, some control sample granularity by the method for test sieving using after gradually grinding repeatedly, are not easy to operate.
Sample granularity is controlled somewhat by the method for lengthening milling time, sample easily occurs into cake, balling phenomenon, causes viscous pot serious
The cleaning of sample difficulty.Agglomeration occurs in some during vibro-grinding, not only granularity is caused not reach requirement, and sample is not
Uniformly.Therefore, powder pressing method sample making technology makes Xray fluorescence spectrometer being of limited application in ferroalloy field.Due to
In ferroalloy analysis field because being influenced by sample technology of preparing, x ray fluorescence spectrometry is widely used in measurement ferroalloy
At home and abroad belong to the stage of fumbling.
Summary of the invention
To solve disadvantage existing in the prior art, the present invention provides the pressed powder system of a kind of ferroalloy productor and raw material
Quadrat method, sample pass through broken and division, chemical analysis sample processed and drying；With its spectrum press sheet compression processed, standard is finally pressed
The round print of specification.It can be adapted to the measurement of energy dispersion type Xray fluorescence spectrometer to require, and guarantee entirely making
Viscous pot and agglomeration do not occur during sample.
In order to solve the above-mentioned technical problem, the pressed powder method for making sample of a kind of ferroalloy productor of the present invention and raw material is specific
Steps are as follows:
Step (1) sample for chemical analysis processed and drying
Inner quality standard sample or sample that crushing division is selected for chemical Par value are weighed, spreads loading grind box out
Inside and outside impact ring, material sample need to be uniformly distributed dropwise addition dehydrated alcohol on sample, then all in required time in vibrating mill
Upper grinding；
Ground sample for chemical analysis and national standard sample are dried；
When crushing division sample it is overly moist it is excessively viscous cannot sieve, be crushed, division when, can be carried out in the temperature lower than quality comparison
Dry, the degree of crusher and reduction device can be passed freely through by reaching sample；
Step (2) spectrum press sheet compression processed
It weighs dried standard or tested sample for chemical analysis is spread out and is packed into inside and outside grind box impact ring, on sample
Dehydrated alcohol is added dropwise in even distribution, and solid grinding aid need to be added is uniformly sprinkling upon sample inside and outside impact ring for quantitative solid grinding aid
On, the set time is ground using continuous quadratic, the mode that midfeather is no less than 10 seconds is ground on vibrating mill；
Grind box is removed, it is careful to open grind box lid, weighed binder is added in grind box inside and outside impact ring again, is continued
Grinding is uniformly mixed itself and sample, is spectrum press sheet compression；
The round print of step (3) pressure standard specification
Boric acid mold is used on pressure-like machine, a certain amount of spectrum press sheet compression is added in boric acid fringing substrate on tablet press machine,
The tabletting of spectrum press sheet compression is used under the conditions of fixed pressure, dwell time；By print is taken out after setting time release, trimming is scraped
Edge protrusion, ear washing bulb blow down dust, to be measured after mark.
As in the preferred step (1), granularity is crushed to less than 3mm, division conical quartering for bulk sample
Or grid division method carries out, the revolution of vibromill is 1380~1390 revs/min.
The inner quality standard sample or sample of ferroalloy productor chemistry Par value are preferred: 40g ferrosilicon is in chromium steel grind box
Grind 20s；50g specialty metal silicon grinds 60s in chromium steel grind box；60g silicomangan grinds 60s in chromium steel grind box；50g silicon
Evanohm grinds 15s in manganese steel grind box；60g high carbon ferro-chrome grinds 60s in manganese steel grind box.The dry temperature of electric drying oven with forced convection
105~110 DEG C of degree, 10~15min of time.
The inner quality standard sample or sample of chemically definite value are preferred: 60g ferriferous raw material is in tungsten carbide grind box
10~12 drop dehydrated alcohols are added dropwise and grind 60s；5~6 drop dehydrated alcohol grinding 30s are added dropwise in 35g silica in tungsten carbide grind box；
10~12 drop dehydrated alcohol grinding 20s are added dropwise in 50g chromite in tungsten carbide grind box；50g manganese ore is added dropwise in tungsten carbide grind box
10~12 drop dehydrated alcohols grind 30s.105~110 DEG C of electric drying oven with forced convection drying temperature, time 2h.
As in the preferred step (2), the revolution of vibromill is 1380~1390 revs/min.
Dry ferroalloy productor standard or tested sample for chemical analysis are preferred: 25.00g ferrosilicon drips in chromium steel grind box
Add 5~6 drop dehydrated alcohol grinding 60+60s, 5.00g boric acid (crossing 40 meshes) binder grinds 10s；20.00g specialty metal silicon
5~6 drop dehydrated alcohols are added dropwise in chromium steel grind box and grind 60s, 6.00g boric acid (crossing 40 meshes) binder grinds 10s；25.00g
10~12 drop dehydrated alcohol grinding 90+90s, 3.00g boric acid (crossing 40 meshes) binder is added dropwise in silicomangan in chromium steel grind box
Grind 10s；5~6 drop dehydrated alcohols are added dropwise in 30.00g silicochromium in manganese steel grind box, and 1.00g methylcellulose binder is ground
Grind 90s；5~6 drop dehydrated alcohol grinding 60+60s are added dropwise in 35.00g high carbon ferro-chrome in manganese steel grind box, and 5.00g boric acid (crosses 40 mesh
Sieve) binder grinding 10s.
Dry raw material standard or tested sample for chemical analysis are preferred: 25.00g ferriferous raw material drips in tungsten carbide grind box
Add 10~12 drop dehydrated alcohol grinding 90+90s, 2.50g microcrystalline cellulose binder grinds 90s；15.00g silica is in tungsten carbide
5~6 drop dehydrated alcohols are added dropwise in grind box, grind 60s, 3.00g starch binder grinds 60s；15.00g chromite is in tungsten carbide
3 drop dehydrated alcohols are added dropwise in grind box, 0.30g Stearic acid solids grinding aid grinds 90s, the grinding of 5.00g microcrystalline cellulose binder
90s；10~12 drop dehydrated alcohols, the grinding of 0.20g Stearic acid solids grinding aid is added dropwise in 15.00g manganese ore in tungsten carbide grind box
60s, 3.00g microcrystalline cellulose binder grind 60s.
As in the preferred step (3), sample amount, which is added, on tablet press machine ensures that thickness will reach 4mm or more, pressure-like machine
Pressure is set as 30t, and the dwell time is set as 30s, and the release time is set as 12s.
Beneficial effect of the present invention
Compared with prior art, generated by adopting the above technical scheme to have the beneficial effect that the iron that invention is tested with us
Alloy product and raw material powder tabletting sample preparation method, substitute current chemical analysis method completely, directly glimmering with energy dispersion type X-ray
Photothermal spectroscopic analyzer analysis ferroalloy productor and the middle Major And Minor Elements of raw material or the chemical component of compound achieve satisfactory point
Analysis is as a result, have no matter certain innovative theoretically or is experimentally to analyze powder to Xray fluorescence spectrometer method
The abundant and development of last tabletting theory and application, has certain theory significance and practical value.
Advantage is in particular in:
1. due to using sample is uniformly first prepared into chemical analysis sample, i.e. ferroalloy productor granularity reaches 120 mesh, former
The granularity of material reaches 180 mesh, then prepares spectrum press sheet compression on the basis of this again.To all samples and standard specimen using standardized
Grinding method makes them substantially there was only identical granularity and size distribution, and the concentration in gradient for realizing chemical Par value becomes
The inner quality standard sample and respective country standard substance of change establish standard curve as calibration sample, imitate the mineral of sample to be tested
The mineral effect of Ying Yinyu standard specimen is consistent and eliminates.
2. selecting effectively suitable grinding aid with the chemical analysis sample accurately weighed, continuous quadratic grinding is rationally controlled
Time, make 200 mesh percent of pass 100% of granularity ferroalloy productor, 300 98% or more mesh percent of pass of raw material penetrates the X of sample
Line fluorescence intensity tends towards stability, and can substantially eliminate the influence of particle.Solves powder particle effect problem by grinding.It is added
Grinding aid not only increases the efficiency of grinding, and due to the peptizaiton of grinding aid, prevents the secondary agglomeration of superfine powder.
3. cooperating the regrinding of optimal proportion binder, it is sufficiently mixed powder sample and binder uniformly, not only makes
It is easy to form when piece, the tabletting of production more rugged strong, structure even compact, available higher bulk density and smooth
Smooth surface；Simultaneously because dilution, reduces absorption-enhancement effect.And sample further crushes, the complete grind box of sample preparation
More easy to clean can be cleaned out with hairbrush.
4. this pressed powder sample preparation method grinds ground sample using mechanical oscillation, electro-hydraulic press pressure-like, sample preparation is high-efficient, adopts
It is reproducible convenient for control with Research of standard programme of posterior process.Labor intensity is lower and of less demanding to operator.
5. investigation situation is carried out to sample preparation effect and is seen according to standard curve regression effect and actual measured results, best item
Part reduces mineral effect and the granularity effect deviation caused by analysis result, carries out matrix effect, spectral line using empirical coefficient method
The correction of overlapping interference and Matrix effects, curve linear relationship is good, guarantees that analysis data are accurate and reliable, analyzes data error control
System is within the scope of national standard tolerance.
Specific embodiment:
With specific embodiment, the invention will be further described below, but the invention is not limited to these embodiments.
X-ray fluorescence analyzer is a kind of relative measurement instrument, it is the standard by measuring certain amount known results
Sample just can be measured accurately after establishing corresponding correctly mathematical model.Therefore Xray fluorescence spectrometer application is applied
When software editing analysis method, select one group of accurate definite value of constituent content chemical method inner quality standard sample, it is each mainly at
Part covers the variation range of each main ingredient in actual production under normal circumstances, and the content of each main ingredient pulls open certain gradient
And it is evenly distributed.The round print of the standard specification of concerned countries standard sample is suppressed simultaneously, participates in drawing standard working curve,
On the one hand on the other hand supplement chemical method verifies the accuracy of analysis method temporarily without the constituent content of Par value.
Embodiment 1: ferrosilicon sample powder tabletting method for making sample and verifying
Broken and division: a step uses jaw crusher to bulk sample, outlet grain size setting is after broken for the first time
All sample granularities are respectively less than 6mm, and are all left to 8~10kg by division with conical quartering.Second broken using Hubei Province formula
Broken machine outlet grain size setting all sample granularities after broken are respectively less than 3mm, and are all left to by division with conical quartering
1.0~2.0kg.Entire sample making course will carry out the facilities such as jaw crusher with a certain amount of pass through three times with batch Antaciron
Thorough cleaning, all samples use identical operating method.
B step, chemical analysis sample processed and drying: the broken sample with division of 40g is weighed, spreads out and is packed into chromium steel grinding box
Inside and outside impact ring, grinding box is firmly clamped on positioning disk, is closed the door carefully.The setting grind away time is 20s, and being pre-adjusted improvement speed is
1380~1390 revs/min, the sample for chemical analysis of preparation is numbered in starting device grinding, dry in 105~110 DEG C of electric heating air blast
Dry 10~15min in dry case dress, dries 30min for national standard sample under identical condition, is placed in cold in drier
But spare to room temperature.Entire sample making course with it is a certain amount of with batch Antaciron thoroughly clean grinding box, impact ring, impact block,
The facilities such as hairbrush, all samples use identical operating method.
Spectrum press sheet compression processed: step c weighs the production standard sample or national standard sample of 25.00g chemistry Par value
Or tested chemical analysis sample, it spreads out and is packed into inside and outside grinding box impact ring, dropwise addition 5~6 is uniformly distributed on sample and drips anhydrous second
Grinding box is firmly clamped on positioning disk, closes the door carefully by alcohol.The setting grind away time is 60s, be pre-adjusted improvement speed for 1380~
1390 revs/min, starting device grinds two 60s, and midfeather is no less than 10 seconds.Grind box is removed, it is careful to open grind box lid, again
5.00g boric acid (crossing 40 meshes) will be weighed to be added in grind box inside and outside impact ring, continue to grind 10s, the light that will be prepared in grind box
It composes tabletting sample and clears up pack number with hairbrush.Entire sample making course with it is a certain amount of with batch Antaciron thoroughly clean grinding box,
The facilities such as impact ring, impact block, hairbrush, all samples use identical operating method.
Step d presses the round print of standard specification: boric acid mold is used on pressure-like machine, boric acid fringing substrate presses model machine
Operation instructions operation, wherein 5~6g ferrosilicon standard sample or sample to be tested spectrum tabletting sample, pressure-like machine pressure are added in hopper
Power is set as 30t, and the dwell time is set as 30s, and the release time is set as 12s,.Print is taken out after release, scrapes off edge projection, is washed
Ear ball blows down dust, to be measured after mark.
Step e, the measurement of element fluorescence intensity to be measured and the calibration of Element detection working curve to be measured: what starting had been edited
Analysis method successively measures the round sample of the standard specification of the production standard sample and national standard sample according to Step d preparation
Piece calibrates corresponding standard according to the content of elements Si to be measured, Al, P, Ca, Ti, Cr, Mn, Fe fluorescence intensity input corresponding element
Analyze working curve.
F step, return and survey sample to be tested and detection: the standard analysis working curve of the drafting according to step e is to tested
Sample analysis measurement is intended to measure Si, Al, P, Ca, Ti, Cr, Mn, Fe content in ferrosilicon sample to be measured, prepares according to step a, b, c, d
Then the round print of associated sample standard specification calls step e standard analysis working curve to analyze ferrosilicon sample to be measured
Middle Si, Al, P, Ca, Ti, Cr, Mn, Fe content.
The test of above method preci-sion and accuracy is as follows:
One inner quality standard sample of precision test, the round print that powder pressing method prepares 10 standard specifications are gone forward side by side
Row measurement, inspection method precision, test data see attached list 1；The round print of one of standard specification is selected to repeat to survey again
Amount 10 times, the precision of testing instruments analysis method, test data sees attached list 2.By subordinate list 1 and 2 test result of subordinate list as it can be seen that originally
Pressed powder technical method and analysis data reappearance are good；Simultaneously by subordinate list 1 it can be seen that the pressed powder method for making sample weight
Existing property is good.
The precision test data of 1 embodiment of table, 1 verification method are as shown in the table
The precision test data of 2 embodiment of subordinate list, 1 validation instrument
Accuracy test: this law selects 5 ferrosilicon national standard samples to carry out accuracy validation, by the test in subordinate list 3
It is preferable that data result shows that measured value meets with standard value.In addition 6 ferrosilicon production sample this laws and national standard method are selected
Accuracy Control is carried out, comparing result is attached to be shown in Table 4, and data result can be seen that this law measurement result and national standard side from subordinate list 4
Method measurement result accordance is fine.
3 embodiment of subordinate list, 1 verification method accuracy test data
4 embodiment of subordinate list, 1 verification method accuracy test data
Embodiment 2: silica sample powder tabletting method for making sample and verifying
A step produces standard sample or sample is crushed and division: first using Hubei Province formula for the first time to the bulk sample of inspection
Crusher just broken not division, uses jaw crusher for the second time, and outlet grain size setting all sample granularities after broken are respectively less than
6mm, and 8~10kg is all left to by division with conical quartering.Third time is existed using the setting of jaw crusher outlet grain size
All sample granularities are respectively less than 3mm after broken, and are all left to 1.0~2.0kg by division with conical quartering.Entire sample preparation
Process will carry out thorough cleaning, all samples to facilities such as jaw crushers three times with a certain amount of pass through with batch silica sample
Using identical operating method.
B step produces the preparation and processing of standard sample or sample chemical analysis sample: weighing 35g and is crushed and contracts
The sample divided is spread out and is packed into inside and outside tungsten carbide grinding box impact ring, and dropwise addition 5~6 is uniformly distributed on sample and drips dehydrated alcohol, is ground
Grind box is firmly clamped on positioning disk, is closed the door carefully.The setting grind away time be 30s, be pre-adjusted improvement speed for 1380~1390 turns/
Point, the sample for chemical analysis of preparation is numbered in starting device grinding, dry in 105~110 DEG C of electric drying oven with forced convection dresses
2h, for national standard sample under identical condition dry 2h, be placed in drier be cooled to room temperature it is spare.Entire sample preparation
Journey thoroughly cleans the facilities such as grinding box, impact ring, impact block, hairbrush with batch silica sample with a certain amount of, and all samples use phase
Same operating method.
Step c, standard sample or the preparation of sample spectrum press sheet compression: the production mark of 15.00g chemistry Par value is weighed
Quasi- sample or national standard sample or tested chemical analysis sample are spread out and are packed into inside and outside grinding box impact ring, on sample uniformly
5~6 drop dehydrated alcohols are added dropwise in distribution, and grinding box is firmly clamped on positioning disk, is closed the door carefully.The setting grind away time is 60s, in advance
First regulating revolving speed is 1380~1390 revs/min, starting device grinding.Grind box is removed, it is careful to open grind box lid, it will be weighed
3.00g starch is added in grind box inside and outside impact ring, continues to grind 60s, and the spectrum tabletting sample hairbrush prepared in grind box is clear
Reason pack number.
Step d prepares the round print of the standard specification of standard sample and sample to be tested: boric acid mould is used on pressure-like machine
Tool, pressing model machine operation instructions operation, wherein 4~5g silica standard sample or sample to be tested spectrum tabletting are added in hopper
Sample, pressure-like machine pressure are set as 30t, and the dwell time is set as 30s, and the release time is set as 12s, boric acid fringing substrate.It is taken out after release
Print, scrapes off edge projection, and ear washing bulb blows down dust, to be measured after mark.
Step e, the measurement of element fluorescence intensity to be measured and the calibration of Element detection working curve to be measured: what starting had been edited
Analysis method successively measures the round sample of the standard specification of the production standard sample and national standard sample according to Step d preparation
Piece, according to elements Si 0 to be measured2、Fe2O3、Al2O3、Ca0、P2O5、TiO2、Mn0、Na2O、K2O fluorescence intensity inputs corresponding element
Content calibrates corresponding standard analysis working curve.
F step, return and survey sample to be tested and detection: the standard analysis working curve of the drafting according to step e is to tested
Sample analysis measures Si0 in silica sample to be measured2、Fe2O3、Al2O3、Ca0、P2O5、TiO2、Mn0、Na2O、K2O content, according to step
The round print of rapid a, b, c, d preparation associated sample standard specification, then calls the analysis of step e standard analysis working curve to be measured
Si0 in silica sample to be measured2、Fe2O3、Al2O3、Ca0、P2O5、TiO2、Mn0、Na2O、K2O content.
The test of above method preci-sion and accuracy is as follows:
Precision test is gone forward side by side with the round print of a silica inner quality standard sample powder pressed disc method preparation standard specification
Row measurement, inspection method precision, test data see attached list 5；The round print of one of standard specification is selected to repeat to survey again
Amount 10 times, the precision of testing instruments analysis method, test data sees attached list 6.By table attached 5 and 6 test result of subordinate list as it can be seen that originally
Pressed powder technical method and analysis data reappearance are good；Simultaneously by subordinate list 6 it can be seen that the pressed powder method for making sample weight
Existing property is good.
The precision test data of 5 embodiment of subordinate list, 2 verification method
The precision test data of 6 embodiment of subordinate list, 2 validation instrument
Accuracy test: this law selects 5 silica national standard samples to carry out accuracy validation, by the test in subordinate list 7
It is preferable that data result shows that measured value meets with standard value.In addition 6 production sample this laws of silica and national standard method are selected
Accuracy Control is carried out, comparing result sees attached list 8, and data result can be seen that this law measurement result and national standard side from subordinate list 8
Method measurement result accordance is fine.
The accuracy test data of 7 embodiment of subordinate list, 2 verification method
The accuracy test data of 8 embodiment of subordinate list, 2 verification method
Claims (8)
1. the pressed powder method for making sample of a kind of ferroalloy productor and raw material, which is characterized in that specific step is as follows:
Step (1) sample for chemical analysis processed and drying
Inner quality standard sample or sample that crushing division is selected for chemical Par value are weighed, spreads out and is packed into grind box impact
Inside and outside ring, material sample need to be uniformly distributed dropwise addition dehydrated alcohol on sample, then all grind on vibrating mill in required time
Mill；
Ground sample for chemical analysis and national standard sample are dried；
When crushing division sample it is overly moist it is excessively viscous cannot sieve, be crushed, division when, can be done in the temperature lower than quality comparison
Dry, the degree of crusher and reduction device can be passed freely through by reaching sample；
Step (2) spectrum press sheet compression processed
It weighs the standard pre-processed or tested sample for chemical analysis is spread out and is packed into inside and outside grind box impact ring, on sample uniformly
Dehydrated alcohol is added dropwise in distribution, need to be added solid grinding aid quantitative solid grinding aid is uniformly sprinkling upon inside and outside impact ring sample it
On, the set time is ground using continuous quadratic, the mode that midfeather is no less than 10 seconds is ground on vibrating mill；
Grind box is removed, it is careful to open grind box lid, weighed binder is added in grind box inside and outside impact ring again, continues to grind
It is uniformly mixed itself and sample, is spectrum press sheet compression；
The round print of step (3) pressure standard specification
Boric acid mold is used on pressure-like machine, a certain amount of spectrum press sheet compression is added in boric acid fringing substrate on tablet press machine, solid
Fixed pressure uses the tabletting of spectrum press sheet compression under the conditions of the dwell time；By print is taken out after setting time release, it is prominent to scrape off edge
Part out, ear washing bulb blow down dust, to be measured after mark.
2. the pressed powder method for making sample of a kind of ferroalloy productor according to claim 1 and raw material, which is characterized in that step
Suddenly in (1), preferably 40g ferrosilicon grinds 20s in chromium steel grind box；50g specialty metal silicon grinds 60s in chromium steel grind box；60g silicon
Manganese alloy grinds 60s in chromium steel grind box；50g silicochromium grinds 15s in manganese steel grind box；60g high carbon ferro-chrome is ground in manganese steel
60s is ground in box.Prepare the inner quality standard sample of ferroalloy productor chemistry Par value or the sample for chemical analysis of sample.
3. the pressed powder method for making sample of a kind of ferroalloy productor according to claim 1 and raw material, which is characterized in that step
Suddenly in (1), preferably 10~12 drop dehydrated alcohol grinding 60s are added dropwise in 60g ferriferous raw material in tungsten carbide grind box；35g silica is in carbon
Change and 5~6 drop dehydrated alcohols grinding 30s are added dropwise in tungsten grind box；10~12 anhydrous second of drop are added dropwise in 50g chromite in tungsten carbide grind box
Alcohol grinds 20s；10~12 drop dehydrated alcohol grinding 30s are added dropwise in 50g manganese ore in tungsten carbide grind box.Prepare chemically definite value
Inner quality standard sample or sample sample for chemical analysis.
4. the pressed powder method for making sample of any one ferroalloy productor according to claim 1 to 3 and raw material, feature
Be, in step (1), electric drying oven with forced convection be arranged 105~110 DEG C of temperature, the inner quality standard sample of chemical Par value or by
Ferroalloy productor 10~15min of drying time of sample, national standard ferroalloy productor drying time 30min, material sample
Drying time 2h.
5. the pressed powder method for making sample of a kind of ferroalloy productor according to claim 1 and raw material, which is characterized in that institute
It states in step (2), preferably 5~6 drop dehydrated alcohol grinding 60+60s, 5.00g boric acid is added dropwise in 25.00g ferrosilicon in chromium steel grind box
(crossing 40 meshes) binder grinds 10s；5~6 drop dehydrated alcohol grindings are added dropwise in 20.00g specialty metal silicon in chromium steel grind box
60s, 6.00g boric acid (crossing 40 meshes) binder grinds 10s；10~12 drop nothings are added dropwise in 25.00g silicomangan in chromium steel grind box
Water-ethanol grinds 90+90s, and 3.00g boric acid (crossing 40 meshes) binder grinds 10s；30.00g silicochromium is in manganese steel grind box
5~6 drop dehydrated alcohols are added dropwise, 1.00g methylcellulose binder grinds 90s；35.00g high carbon ferro-chrome drips in manganese steel grind box
Add 5~6 drop dehydrated alcohol grinding 60+60s, 5.00g boric acid (crossing 40 meshes) binder grinds 10s.Prepare ferroalloy productor mark
Quasi- or tested spectrum press sheet compression.
6. the pressed powder method for making sample of a kind of ferroalloy productor according to claim 1 and raw material, which is characterized in that institute
It states in step (2), preferably 10~12 drop dehydrated alcohol grinding 90+90s are added dropwise in 25.00g ferriferous raw material in tungsten carbide grind box,
2.50g microcrystalline cellulose binder grinds 90s；5~6 drop dehydrated alcohols, grinding is added dropwise in 15.00g silica in tungsten carbide grind box
60s, 3.00g starch binder grind 60s；3 drop dehydrated alcohols are added dropwise in 15.00g chromite in tungsten carbide grind box, and 0.30g is hard
Resin acid solid grinding aid grinds 90s, and 5.00g microcrystalline cellulose binder grinds 90s；15.00g manganese ore drips in tungsten carbide grind box
Add 10~12 drop dehydrated alcohols, 0.20g Stearic acid solids grinding aid grinds 60s, and 3.00g microcrystalline cellulose binder grinds 60s.
Prepare raw material standard or tested spectrum press sheet compression.
7. the pressed powder method for making sample of any one ferroalloy productor and raw material described in -6 according to claim 1, feature
It is, in step (1) and (2), the revolution of vibromill is set as 1380~1390 revs/min.
8. the pressed powder method for making sample of a kind of ferroalloy productor according to claim 1 and raw material, which is characterized in that institute
It states in step (3), sample amount is added on tablet press machine ensures that thickness will reach 4mm or more, and pressure-like machine pressure is set as 30t, when pressure maintaining
Between be set as 30s, the release time is set as 12s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114371186A (en) * | 2022-01-07 | 2022-04-19 | 鞍钢股份有限公司 | Method for overcoming grain size effect of alloy elements determined by XRF powder tabletting method |
| CN114577834A (en) * | 2022-05-06 | 2022-06-03 | 广东省农业科学院动物科学研究所 | Aquatic product quality detection method based on X-ray fluorescence spectrum analysis |
| CN114778247A (en) * | 2022-04-26 | 2022-07-22 | 鞍钢集团矿业有限公司 | Preparation method of iron ore sample tablet for detection of fluorescence analyzer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076351A (en) * | 2012-12-27 | 2013-05-01 | 天津钢管集团股份有限公司 | Method for measuring Mo element in tungstenic ferro-molybdenum alloy through X-ray fluorescence spectrum analysis |
| CN103389232A (en) * | 2012-05-07 | 2013-11-13 | 广东韶钢松山股份有限公司 | Powder alloy cast iron X-ray fluorescence spectral analysis sample preparation method |
| CN104020032A (en) * | 2014-06-17 | 2014-09-03 | 攀钢集团攀枝花钢钒有限公司 | Preparation method of test specimens for unbreakable ferro-vanadium chemical analysis |
| CN105866154A (en) * | 2016-03-31 | 2016-08-17 | 天津渤化永利化工股份有限公司 | Method for determining ferroalloy by using powder compressed tablet |
-
2018
- 2018-02-07 CN CN201810121492.8A patent/CN110118792A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389232A (en) * | 2012-05-07 | 2013-11-13 | 广东韶钢松山股份有限公司 | Powder alloy cast iron X-ray fluorescence spectral analysis sample preparation method |
| CN103076351A (en) * | 2012-12-27 | 2013-05-01 | 天津钢管集团股份有限公司 | Method for measuring Mo element in tungstenic ferro-molybdenum alloy through X-ray fluorescence spectrum analysis |
| CN104020032A (en) * | 2014-06-17 | 2014-09-03 | 攀钢集团攀枝花钢钒有限公司 | Preparation method of test specimens for unbreakable ferro-vanadium chemical analysis |
| CN105866154A (en) * | 2016-03-31 | 2016-08-17 | 天津渤化永利化工股份有限公司 | Method for determining ferroalloy by using powder compressed tablet |
Non-Patent Citations (3)
| Title |
|---|
| 周西林 等主编: "《原子光谱仪器操作入门》", 31 August 2015, 国防工业出版社 * |
| 张东雯 等: "全自动制样－Ｘ射线荧光光谱法测定硅铁中硅", 《冶金分析》 * |
| 邱少花 等: "粉末压片制样—X 射线荧光光谱法测定钼铁中的钼", 《中国钼业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114371186A (en) * | 2022-01-07 | 2022-04-19 | 鞍钢股份有限公司 | Method for overcoming grain size effect of alloy elements determined by XRF powder tabletting method |
| CN114371186B (en) * | 2022-01-07 | 2024-03-19 | 鞍钢股份有限公司 | Method for overcoming particle size effect of alloy element measured by XRF powder tabletting method |
| CN114778247A (en) * | 2022-04-26 | 2022-07-22 | 鞍钢集团矿业有限公司 | Preparation method of iron ore sample tablet for detection of fluorescence analyzer |
| CN114577834A (en) * | 2022-05-06 | 2022-06-03 | 广东省农业科学院动物科学研究所 | Aquatic product quality detection method based on X-ray fluorescence spectrum analysis |
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