CN110261420A - The method of x-ray fluorescence spectrometry serpentine chemical component - Google Patents
The method of x-ray fluorescence spectrometry serpentine chemical component Download PDFInfo
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- CN110261420A CN110261420A CN201910599716.0A CN201910599716A CN110261420A CN 110261420 A CN110261420 A CN 110261420A CN 201910599716 A CN201910599716 A CN 201910599716A CN 110261420 A CN110261420 A CN 110261420A
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- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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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Abstract
The invention discloses it is a kind of with X fluorescence spectrum method measurement serpentine in silica, magnesia, aluminum oxide content method.Compared with existing detection technique, the present invention uses x ray fluorescence spectrometry, and it is complicated for operation to overcome original wet chemical analysis method, and analysis time is long, big using amount of reagent, the defects of easily polluting the environment, multielement simultaneous determination is realized, reagent dosage is few, the technological break-through of safe operation environmental protection, it is fast with analysis speed, sample melted sheet glass retention time is long, and analytical precision, accuracy are high, is suitble to the demand that scene is quickly analyzed in Production Process for Steel Enterprise.
Description
Technical field
The invention belongs to technical field of analysis and detection, and in particular to a kind of x-ray fluorescence spectrometry serpentine chemistry
SiO in the method for ingredient more particularly to a kind of x-ray fluorescence spectrometry serpentine2、MgO、Al2O3Content.
Background technique
Serpentine is the group name of silicate mineral, and chemical formula is (Mg, Fe)3Si2O5(OH)4, main component two
Silica, magnesia, aluminum oxide etc., quality account for about the 70%~80% of serpentine.
Magnesia in serpentine can be used as the flux in ironmaking processes, and in slagging process, suitable magnesia contains
Amount can improve the mobility and stability of clinker, be conducive to keep furnace condition anterograde, improve slag desulfurization, be the one of blast furnace ironmaking
The important auxiliary material of kind；Simultaneous oxidation magnesium, silica and a small amount of aluminum oxide etc. are the primary of influence blast furnace basicity again
Element, therefore it provides a kind of accuracy is high, easy to operate, the quick serpentine chemical component measuring method of analysis is currently to examine
Survey the urgent need of industry.
The measurement of silica, magnesia, aluminum oxide in serpentine, generally use traditional chemical analysis method into
Row analysis.Silica is evaporated determination using classical secondary hydrochloric acid, and magnesia, aluminum oxide use EDTA capacity
Method.Since the sample handling processes of these methods are cumbersome, analysis time is long, it is unable to multielement simultaneous determination, is unable to satisfy at present
The needs quickly produced.
The content of background technology part is only the technology that inventor is known, not the existing skill of natural representative this field
Art.
Summary of the invention
One or more aiming at the problems existing in the prior art, the present invention provide a kind of x ray fluorescence spectrometry survey
Determine silica in serpentine, magnesia, aluminum oxide content method, comprising the following steps:
S1: the series standard sample that ingredient content range has concentration gradient is prepared using serpentine standard sample；
S2: by prepared series standard sample and sample to be tested respectively with mixed flux after mixing, be added demoulding
Series standard print and test piece to be measured is prepared in agent, high-temperature fusion；
S3: using Xray fluorescence spectrometer under the measuring condition set, serial standard sample of photo is detected, using PCMXF
Software obtains the calibration curve of element silica to be measured, magnesia, the intensity value of aluminum oxide and relation with contents；
S4: detecting test piece to be measured using Xray fluorescence spectrometer under the measuring condition of S3, bent according to the calibration of S3
Line obtains the content of silica, magnesia, aluminum oxide in serpentine.
Before step S1, high temperature sintering also is carried out to serpentine standard sample and sample to be tested, the high temperature sintering
Method particularly includes: suitable serpentine standard sample is weighed respectively and sample to be tested is placed in constant weight container, in 950 ± 10 DEG C of horses
Not calcination lh, taking-up are cooled to room temperature in furnace, are placed in spare in drier.
Above-mentioned serpentine standard sample is GBW (E) 070201 serpentine standard sample.
The concrete operation method of above-mentioned steps S1 are as follows: 12 different serpentine standard samples of quality are weighed respectively, as
Calibration standard sample to be measured, using 0.7000g standard sample as basic sample weighting amount, weighed calibration standard sample quality to be measured with
0.7000g compares, asserting value of the component content being converted into as component content in the calibration standard sample to be measured, conversion at
Point content range should be able to cover in actual use component content range in serpentine；Specific convert formula are as follows: calibration to be measured
The component content asserting value of standard sample=(component content in the basic sample weighting amount of quality * of weighed calibration standard sample to be measured
Asserting value)/0.7000.
In above-mentioned steps S2, the mixed flux is the mixture of lithium metaborate and anhydrous lithium tetraborate, and mass ratio is
33%:67%.
In above-mentioned steps S2, the mass ratio of the series standard sample and sample to be tested and mixed flux is 1:1.1.
In above-mentioned steps S2, the release agent is lithium bromide, mass percent concentration 10%.
In above-mentioned steps S2, the high-temperature fusion uses high temperature smelting furnace, and melting temperature is 1050 DEG C ± 10 DEG C, when melting
Between include static heating melting, wave heating melting and rotary heating melting time, amount to 20min.
In above-mentioned steps S3, according to the detection range for the calibration curve that series standard sample is drawn are as follows: SiO2:
25.00% -45.00%；MgO:25.00% -45.00%；AL2O3: 0.50% -2.00%.
Silica in serpentine, oxidation are detected with X-ray fluorescence spectra analytic approach based on what above technical scheme provided
The content of magnesium, aluminum oxide, with easy to operate, multielement simultaneous determination, analysis is quick, result is accurate, and precision height etc. is excellent
Point；High-temperature fusion method for making sample is used simultaneously, eliminates matrix and the interference of granularity difference bring, and use an only snake
Line stone standard sample converts ratio according to different quality, has synthesized series of calibration standard sample, has solved serpentine standard sample
Product are few, draw the problem of calibration curve difficulty.Glass melting piece can also save for a long time simultaneously, reduce labor intensity, contract
Short analysis time, improve analysis efficiency.
Compared with prior art, the present invention realizes the skill of multielement simultaneous determination in serpentine using x-ray fluorescence method
Art is broken through.Due to SiO in serpentine2、MgO、Al2O3Content is different, SiO2, content of MgO it is higher, Al2O3Content is low, needs to select
Suitable mixed flux can just take into account the requirement of different content, different elements melts, and by test, selecting mass ratio is 33%:
67% lithium metaborate and the mixed flux of anhydrous lithium tetraborate, with sample to be tested with 1.1:1 mass ratio, at 1050 DEG C ± 10 DEG C
20min is melted in high temperature smelting furnace, the sample melten glass piece of preparation can long-term preservation；Simultaneously according to the series standard sample of synthesis
The calibration curve that product are drawn, SiO in the serpentine of detection2、MgO、Al2O3Content, quality meet production needs.This method
It overcomes and is unable to simultaneous determination of multiponents and the few defect of standard sample existing for original wet chemical analysis method, there is analysis
Speed is fast, easy to operate, Environmental Safety, melten glass piece storage life limit for length, testing result precision height and good excellent of accuracy
Point can be widely applied to the detection and analysis of serpentine in iron and steel enterprise's smelting process.
Detailed description of the invention
Fig. 1 is the calibration curve graph of silica；
Fig. 2 is the calibration curve graph of magnesia；
Fig. 3 is the calibration analysis graph of aluminum oxide.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of this its protection scope.
Embodiment 1:
The present embodiment provides a kind of methods of chemical component in x-ray fluorescence spectrometry serpentine comprising following
Step:
S1: the drying of standard sample and sample to be tested: by serpentine standard sample, (number is the snake of GBW (E) 070201
Stone) and prior to 105 DEG C baking ovens of sample to be tested in dry be put into drier after a hour it is cooling, it is stand-by after being cooled to room temperature.
S2: high temperature sintering standard sample: serpentine standard sample 15g, 2-3g sample to be tested is accurately weighed, perseverance is respectively placed in
In the container (containers such as cupel or platinum crucible) of weight, to constant weight (general lh), taking-up is set for calcination in 950 ± 10 DEG C of Muffle furnaces
It in drier, is cooled to room temperature, weighs and records, while calculating igloss COEFFICIENT K, and the quality ÷ sample after K=sample calcination
Quality before product calcination.
Due to the commercially available serpentine standard sample that only one number is GBW (E) 070201 at present, using X fluorescence spectrum
Analyzing serpentine chemical component needs the working curve drawn using serial serpentine standard sample to carry out unknown sample ingredient
Detection, needing to synthesize using only serpentine standard sample, there is the series of calibration standard sample of certain ingredients concentration gradients to use
In drafting calibration curve.It to weigh 15g in advance thus and number the serpentine standard sample for being GBW (E) 070201 in high temperature
It is spare after calcination.
S3: the synthesis of series of calibration standard sample
Since domestic serpentine standard sample is less, at present only one number be GBW (E) 070201 serpentine standard
Sample can only prepare the series of calibration standard sample for drawing calibration curve using the method for quality conversion.Concrete operations are as follows: will compile
Number 12 are weighed respectively not after high temperature sintering as basic standard sample for the serpentine standard sample of GBW (E) 070201
The basic standard sample of homogenous quantities claims sample using 0.7000g basic standard sample as basic as calibration standard sample to be measured
Amount, weighed calibration standard sample quality to be measured is compared with 0.7000g, and the content being converted into is as the calibration standard sample to be measured
Asserting value, the component content range of conversion should be able to cover in actual use component content range in serpentine.Specific folding
Calculate formula are as follows: the component content asserting value of calibration standard sample to be measured=(the quality * of weighed calibration standard sample to be measured is basic
Component content asserting value in sample weighting amount)/0.7000.
The series of calibration standard sample actually prepared: according to the content of daily serpentine sample, according to certain sample weighting amount,
It is configured to the series of calibration standard sample with certain concentration gradients.Series of calibration standard sample sample weighting amount, each object being configured to
The content distribution table of matter and ingredient is shown in Table 1.
Series of calibration standard sample sample weighting amount, each substance and the component content distribution table that table 1 is configured to
Note: component content/(1- calcination loss amount) * 100% before component content=calcination after calcination
S4: the preparation of glass melting piece
The preparation of the glass melting piece of series of calibration standard sample and sample to be tested: the synthesis series of calibration designed according to S3
The sample weighting amount of standard sample accurately weighs 12 mark number GBW (E) 070201 serpentine standard samples crossed by high temperature sintering,
0.7000g ± 0.0001g sample to be tested is transferred to respectively in the platinum crucible of different numbers, and the 7.7000g accurately weighed is added
± 0.0001g mixed flux (33%LiBO2+ 67%Li2B4O7) flux mixing, after mixing, 4 drop lithium bromides of addition
(10%) solution is put into and has warmed up into 1050 DEG C of high temperature smelting furnace, according to static heating melting, waves heating melting and rotation
Turn the heating method of heating melting, the automatic heating melting 20min of setting program, to sample melted after, be cooled to room temperature, will
Manufactured glass melting piece is poured out, it is labelled be put into it is spare in drier.Answer smooth, nothing in the glass melting piece surface prepared
Bubble, it is flawless, it is representative.High temperature smelting furnace heating parameters are shown in Table 2.
2 high temperature smelting furnace heating parameters of table
| Static heating method | Wave heating method | Rotary heating mode |
| 5min | 1min | 14min |
S5: calibration curve is drawn
To the series of calibration standard sample glass melting piece (standard sample of photo) of S4 preparation, using X-ray fluorescence spectra
Instrument carries out the measurement of intensity under the best luminoscope measuring condition set, and using PCMXF software, it is dry to carry out overlap of spectral lines
After disturbing correction and matrix correction, the calibration curve of silica, magnesia, aluminum oxide, linearly dependent coefficient are obtained
Meet analysis to require；Wherein table 3 is instrumental conditions；Table 4 is the intensity value for the series of calibration standard sample measurement prepared；Table
5 be the running parameter of calibration curve；Fig. 1 is the calibration curve graph of silica；Fig. 2 is the calibration of magnesia
Curve graph；Fig. 3 is the calibration curve graph of aluminum oxide.
3 instrumental conditions of table
The intensity value for the series of calibration standard sample measurement that table 4 is prepared
The running parameter of 5 calibration curve of table
| Element | Linear equation | Related coefficient | Detection range |
| Silica | Y=0.8327X+4.1381 | 0.9988 | 25.00%--45.00% |
| Magnesia | Y=0.1452X+0.3371 | 0.9991 | 25.00%--45.00% |
| Aluminum oxide | Y=0.5929X+0.2926 | 0.9976 | 0.50%--2.00% |
In conjunction with table 5 it is found that the related coefficient of the calibration curve of each element is all 0.997 or more, calibration is bent
Line it is linear good；Detection range covers the content range of practical serpentine sample.
S6: silica in serpentine sample, magnesia, aluminum oxide content composition detection
The sample to be tested melten glass piece (test piece to be measured) being prepared into is put into Xray fluorescence spectrometer, is marked with calibration
The x ray fluorescence spectrometry calibration curve that quasi- print is established measures, after Xray fluorescence spectrometer detects, automatically
It calculates the content of each ingredient in sample, and by conversion, obtains the content of SiO2, MgO, Al2O3 in primary sample before calcination.
In order to verify the accuracy of this detection method, 4 inspection samples are selected, using the side compared with chemical method
Formula verifies the accuracy of this method.Testing result is shown in Table 6.
6 method accuracy test result of table
As shown in Table 6, chemical score and XRF value compare, and the difference of two methods is smaller, illustrates the accuracy of this detection method
Well.
Precision test: the precision in order to verify this detection method has carried out continuous 10 times identical to same sample
MTG YBCO bulk carries out each component measurement using Xray fluorescence spectrometer, calculates average value, standard deviation and relative standard deviation；
Precision testing result is shown in Table 7.
7 precision testing result (n=10) of table
By the analysis result of table 7 as it can be seen that SiO2、MgO、Al2O3Relative standard deviation all within the scope of lesser, say
Bright this method has good precision.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (9)
1.X ray fluorescence spectrometry measure serpentine in silica, magnesia, aluminum oxide content method, feature
It is, comprising the following steps:
S1: the series standard sample that ingredient content range has concentration gradient is prepared using serpentine standard sample；
S2: by prepared series standard sample and sample to be tested respectively with mixed flux after mixing, release agent is added, it is high
Temperature melting, is prepared series standard print and test piece to be measured；
S3: using Xray fluorescence spectrometer under the measuring condition set, detecting serial standard sample of photo, soft using PCMXF
Part obtains the calibration curve of element silica to be measured, magnesia, the intensity value of aluminum oxide and relation with contents；
S4: detecting test piece to be measured using Xray fluorescence spectrometer under the measuring condition of S3, according to the calibration curve of S3,
Obtain the content of silica, magnesia, aluminum oxide in serpentine.
2. according to the method described in claim 1, it is characterized by: before step S1, also to serpentine standard sample and to
Test specimens carry out high temperature sintering, the high temperature sintering method particularly includes: weigh respectively suitable serpentine standard sample and to
Test specimens are placed in constant weight container, and the calcination lh in 950 ± 10 DEG C of Muffle furnaces, taking-up is cooled to room temperature, and are placed in standby in drier
With.
3. method according to claim 1 or 2, it is characterised in that: the serpentine standard sample is GBW (E) 070201
Serpentine standard sample.
4. method according to any one of claim 1-3, it is characterised in that: the concrete operation method of step S1 are as follows: point
12 serpentine standard samples for also known as taking quality different, as calibration standard sample to be measured, using 0.7000g standard sample as
Basic sample weighting amount, for weighed calibration standard sample quality to be measured compared with 0.7000g, the component content being converted into is to be measured as this
The asserting value of component content in calibration standard sample, the component content range of conversion should be able to cover in actual use in serpentine
Component content range；Specific convert formula are as follows: the component content asserting value of calibration standard sample to be measured=(weighed school to be measured
The asserting value of component content in the basic sample weighting amount of quality * of quasi- standard sample)/0.7000.
5. according to the method described in claim 1, it is characterized by: the mixed flux is lithium metaborate and nothing in step S2
The mixture of water lithium tetraborate, mass ratio 33%:67%.
6. according to the method described in claim 1, it is characterized by: in step S2, the series standard sample and sample to be tested
Mass ratio with mixed flux is 1:1.1.
7. according to the method described in claim 1, it is characterized by: the release agent is lithium bromide, quality percentage in step S2
Specific concentration 10%.
8. according to the method described in claim 1, the high-temperature fusion uses high temperature smelting furnace it is characterized by: in step S2,
Melting temperature is 1050 DEG C ± 10 DEG C, when the melting time includes static heating melting, waves heating melting and rotary heating melting
Between, amount to 20min.
9. according to the method described in claim 1, it is characterized by: in step S3, the calibration drawn according to series standard sample
The detection range of working curve are as follows: SiO2: 25.00% -45.00%；MgO:25.00% -45.00%；AL2O3: 0.50%-
2.00%.
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| CN111855722A (en) * | 2020-07-10 | 2020-10-30 | 南京钢铁股份有限公司 | MgO and SiO in light-burned magnesium and magnesium stone2X-ray fluorescence spectrum analysis method of content |
| CN112362655A (en) * | 2020-09-29 | 2021-02-12 | 新兴铸管股份有限公司 | Crushing mechanism and identification method for cement mortar lining of nodular cast iron pipe fitting |
| CN113899771A (en) * | 2021-09-24 | 2022-01-07 | 同济大学移动源后处理研究院 | Basalt SiO2Content detection method |
| CN113984819A (en) * | 2021-10-08 | 2022-01-28 | 山东莱钢永锋钢铁有限公司 | Raw dolomite high-temperature melting X fluorescence measurement method |
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| CN111855722A (en) * | 2020-07-10 | 2020-10-30 | 南京钢铁股份有限公司 | MgO and SiO in light-burned magnesium and magnesium stone2X-ray fluorescence spectrum analysis method of content |
| CN112362655A (en) * | 2020-09-29 | 2021-02-12 | 新兴铸管股份有限公司 | Crushing mechanism and identification method for cement mortar lining of nodular cast iron pipe fitting |
| CN113899771A (en) * | 2021-09-24 | 2022-01-07 | 同济大学移动源后处理研究院 | Basalt SiO2Content detection method |
| CN113984819A (en) * | 2021-10-08 | 2022-01-28 | 山东莱钢永锋钢铁有限公司 | Raw dolomite high-temperature melting X fluorescence measurement method |
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Application publication date: 20190920 |
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