CN108802084A - X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide - Google Patents
X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide Download PDFInfo
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- CN108802084A CN108802084A CN201810604889.2A CN201810604889A CN108802084A CN 108802084 A CN108802084 A CN 108802084A CN 201810604889 A CN201810604889 A CN 201810604889A CN 108802084 A CN108802084 A CN 108802084A
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention belongs to chemical analysis processing technology field, it is related to method, aluminium hydroxide and its application of component content in a kind of x ray fluorescence spectrometry analysis aluminium hydroxide.The method of component content, includes the following steps in the x ray fluorescence spectrometry analysis aluminium hydroxide of the present invention：Grinding；Pressed powder；Using x ray fluorescence spectrometry, the emissive porwer for measuring each ingredient in print carries out Al in aluminium hydroxide print to be measured using the working curve of established each ingredient2O3、Fe2O3、SiO2And Na2The analysis of O content.The method of the present invention is easy to operate, and analyze speed is fast, can analyze Al in aluminium hydroxide simultaneously2O3、Fe2O3、SiO2、Na2Tetra- ingredients of O, by confirming that this method has the characteristics that science, advance, applicability, analysis time is short, accuracy is high, reproducible, pollution-free；Repeatability and reproducibility is superior to the assay method of chemical composition in the aluminium hydroxide of national standard.
Description
Technical field
The invention belongs to chemical analysis processing technology fields, and hydrogen is analyzed in particular to a kind of x ray fluorescence spectrometry
The method of component content, aluminium hydroxide and its application in aluminium oxide.
Background technology
Aluminium hydroxide is a kind of widely used raw material of industry, can be used for manufacturing drug, fire retardant, waterproof fabric, oil
The fields such as ink, glass.For example, aluminium hydroxide is applied at float glass field, mainly plays and introduce Al2O3The work of ingredient
With, and preparing glass charge calculating need to use aluminium hydroxide chemical composition.The quality of aluminium hydroxide directly affects the ingredient of glass, molding
The performances such as viscosity, physical chemistry；In Improving Glass Manufacturing Processes, the ingredient of aluminium hydroxide is largely transferred among glass, thus hydrogen
The variation of the content of ingredient and ingredient can cause glass ingredient and changes of contents in aluminium oxide, the practical application to glass or use
Performance impacts.Since the main component in aluminium hydroxide includes not only Al2O3, also include Fe2O3、SiO2、Na2The ingredients such as O.
Therefore Accurate Determining goes out main chemical compositions and its content in aluminium hydroxide has certain guidance for the production of float glass
Meaning.
The method of each component content mostly uses following aluminium hydroxide industry relevant criterion in present analysis aluminium hydroxide raw material
(YS/T534.2~534.5) (GB/T6610.2~6610.5) chemical analysis method：
The measurement of loss on ignition (igloss) uses gravimetric method；
The measurement of dioxide-containing silica uses molybdenum blue spectrophotometry；
The measurement of ferric oxide content uses phenanthrolene photometry；
The measurement of sodium oxide content uses flame spectrophotometry/flame atomic absorption spectrometry；
Alundum (Al2O3) content is：100% subtracts the summation of silica, sodium oxide molybdena, di-iron trioxide and igloss amount, i.e.,
w(Al2O3)=100%-w (SiO2)-w(Na2O)-w(Fe2O3)-igloss.
The each project of above-mentioned chemical analysis method needs individually detection, can only individual element analysis, operating process is complicated, sample
Product pre-treatment is complicated, and link is more, is related to that knowledge point is more, and instrumentation difficulty is big, and time-consuming (single sample needs week age), disappears
Consumption reagent is more, is related to harmful influence use, and chemical agent Meteorological is more, while the use of a large amount of drugs also increases pollutant
Discharge, can cause environmental pollution.In addition, what is measured is less reproducible, accuracy as a result is poor, every testing result
(SiO2、Fe2O3、Na2O, the testing result of igloss) error is easy to be superimposed upon Al2O3On.
In consideration of it, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of easy to operate, and sample treatment is simple, and analytical cycle is short, without chemistry
Pollution, accuracy is high, and the method for component content, existing to alleviate in reproducible x ray fluorescence spectrometry analysis aluminium hydroxide
The problem of with the presence of component content in aluminium hydroxide is measured in technology.
The second object of the present invention be to provide it is a kind of by the x ray fluorescence spectrometry analysis aluminium hydroxide at
The aluminium hydroxide obtained after the method analysis of point content.The third object of the present invention is to provide a kind of aluminium hydroxide and exists
As the application in the raw material of production float glass.Method through the invention can be obtained fast and accurately in aluminium hydroxide
The aluminium hydroxide is applied in production float glass, it can be ensured that the component content of glass makes by the inspection data of component content
The quality of glass is guaranteed.
To achieve the above object, the technical solution adopted by the present invention is：
According to an aspect of the present invention, ingredient in a kind of x ray fluorescence spectrometry analysis aluminium hydroxide of present invention offer
The method of content, includes the following steps：
Grinding；
Pressed powder；
Using x ray fluorescence spectrometry, the emissive porwer of each ingredient in print is measured, the work of established each ingredient is utilized
Make curve, carries out Al in aluminium hydroxide print to be measured2O3、Fe2O3、SiO2And Na2The analysis of O content.
As further preferred technical solution, time of grinding is 15~35min, the granularity of the sample ground≤
200 mesh, preferably 80~150 mesh.
As further preferred technical solution, during pressed powder, 30~50MPa of pressure, 20~40s of static pressure.
As further preferred technical solution, the mode for establishing the working curve of each ingredient includes：
There is provided multiple aluminium hydroxide standard samples, Al in each standard sample2O3、Fe2O3、SiO2And Na2Mass ratio shared by O
It is different；
Standard sample is ground respectively and pressed powder, standard sample tabletting is made；
The emissive porwer of each ingredient in bioassay standard sample tabletting is distinguished using Xray fluorescence spectrometer；
By x-ray fluorescence characteristic spectral line intensity and corresponding Al2O3、Fe2O3、SiO2And Na2O mass percentages carry out
Linear regression respectively obtains Al2O3、Fe2O3、SiO2And Na2O corresponds to the standard working curve of x-ray fluorescence characteristic spectral line intensity.
As further preferred technical solution, the quantity of standard sample is >=4.
As further preferred technical solution, time of grinding is 15~35min, the granularity of the sample ground≤
200 mesh, preferably 80~150 mesh；
And/or during pressed powder, 30~50MPa of pressure, 20~40s of static pressure.
As further preferred technical solution, each ingredient in aluminium hydroxide is measured using Xray fluorescence spectrometer to print
Determination condition be respectively：
Al2O3：2 θ 144.65, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal PET, collimator
0.25, PHD40~100, interference element is without sweep time 20s；
Fe2O3：2 θ 57.53, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal LiF200, collimator
0.15, PHD40~100, interference element is without sweep time 20s；
SiO2：2 θ 109.001, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal PET, collimator
0.60, PHD50~95, interference element is without sweep time 12s；
Na2O：2 θ 23.951, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal AX06, collimator
0.60, PHD40~100, interference element is without sweep time 20s.
As further preferred technical solution, the print includes aluminium hydroxide print and standard sample print to be measured.
According to another aspect of the present invention, the present invention provides a kind of by above-mentioned x ray fluorescence spectrometry analysis hydrogen
The aluminium hydroxide obtained after the method analysis of component content in aluminium oxide.
According to another aspect of the present invention, the present invention also provides a kind of aluminium hydroxides as production float glass process glass
Application in the raw material of glass.
Compared with prior art, the beneficial effects of the present invention are：
1, the present invention determines the content of chemical composition in aluminium hydroxide with X-ray fluorescence spectra analytic approach, by hydrogen-oxygen
Change aluminum feedstock to be ground, then direct powder compression sample preparation is directly scanned with X-ray fluorescence spectrometer, measure
The content of chemical composition therein.This method is easy to operate, and analyze speed is fast, can analyze Al in aluminium hydroxide simultaneously2O3、
Fe2O3、SiO2、Na2Tetra- ingredients of O, accuracy is high, reproducible, has filled up with x-ray fluorescence pressed powder analysis test hydrogen
The blank of chemical composition in aluminium oxide.
2, powder pressing method sample preparation of the present invention, operating method is simple, and sample pre-treatments are easy to operate, and analytical cycle is short, fast
Degree is fast, and accuracy is high, and repeatability and reproducibility is superior to the assay method of chemical composition in the aluminium hydroxide in national standard, has
Have that science, advance, applicability, replicability, pollution-free, analysis time is short, accuracy is high, reproducible, nondestructive analysis
The features such as.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiments and examples, but this field skill
Art personnel will be understood that following embodiments and embodiment are merely to illustrate the present invention, and be not construed as the model of the limitation present invention
It encloses.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.The person that is not specified actual conditions, builds according to normal condition or manufacturer
The condition of view carries out.
In a first aspect, providing ingredient in a kind of x ray fluorescence spectrometry analysis aluminium hydroxide at least one embodiment
The method of content, includes the following steps：
Grinding；
Pressed powder；
Using x ray fluorescence spectrometry, the emissive porwer of each ingredient in print is measured, the work of established each ingredient is utilized
Make curve, carries out Al in aluminium hydroxide print to be measured2O3、Fe2O3、SiO2And Na2The analysis of O content.
That X-ray fluorescence spectra analytic approach (XRF) has the characteristics that is accurate, quickly, analyst coverage it is wide, be widely used in ground
The fields such as matter, metallurgy, machine-building, environmental protection, chemical industry, for this method relative to chemical analysis method, sample pre-treatments are simple, chemistry
Reagent dosage is few, and discharge waste is few, and accuracy and precision are high.But there is presently no the complete detection method applications of the method
The measurement of the content of ingredient in aluminum hydroxide material.Based on this, the present invention provides a kind of x ray fluorescence spectrometries to analyze hydrogen
The method of component content in aluminium oxide has been filled up with chemical composition in x-ray fluorescence pressed powder analysis test aluminium hydroxide
Blank.
Present invention chemical composition in X-ray fluorescence spectra assay aluminium hydroxide, is ground aluminium hydroxide
Processing, direct powder compression sample preparation are directly scanned with X-ray fluorescence spectrometer, measure the content of wherein chemical composition, behaviour
Make simply, analyze speed is fast, can analyze Al in aluminium hydroxide simultaneously2O3、Fe2O3、SiO2、Na2Tetra- ingredients of O.The present invention passes through
It is to the characteristics of specificity analysis of aluminium hydroxide sample：Easy to operate, repeatability and reproducibility is superior to the hydrogen-oxygen of national standard
Change the assay method (YS/T534.2~534.5) (GB/T6610.2~6610.5) of chemical composition in aluminium, has scientific, first
Into property, applicability, replicability, analysis time is short, does not have the spies such as chemical contamination, high, the reproducible, nondestructive analysis of accuracy
Point.Further speaking, the opposite component content measured with existing standard chemical method in aluminium hydroxide, the present invention mainly have with
Lower advantage：
(1) economic benefit：The use for having saved a large amount of chemicals, reduces testing cost；It is easy to operate, reduce behaviour
The configuration for making personnel, reduces personnel cost.
(2) Saving in time costs：Sample pre-treatments are simple, quick, can be with multielement simultaneous determination, and a sample analysis is by original
Foreshorten within 1-2 days 1-2 hours, reduce detection time and manpower consumption, detection cycle is short, and it is strong to also solve personnel's labour
Spend big, undermanned problem.
(3) environmental benefit：Greatly reduce the discharge of the use and acid pickle the like waste of poisonous and harmful chemicals, it is acyclic
Border is polluted, and environmental benefit is good.
(4) analytical error is small, and accuracy is high, reproducible, enough fast and accurately can send out inspection data as a result, and
When for production be provided with profit analysis data guidance, it is ensured that finally obtained product quality.
The operation principle of the present invention can be understood as：
For the secondary X-ray that x-ray bombardment generates on substance x-ray fluorescence, each element can radiate correspondence
X-ray fluorescence, measure these radiate come x-ray fluorescence, be converted into the type and content of various elements in sample.
Action relationships：
Grinding → tabletting → Xray fluorescence spectrometer detection
The method of present invention chemical composition in X-ray fluorescence spectra assay aluminium hydroxide, including following technique
Step：Aluminium hydroxide is ground, direct powder compression sample preparation is directly scanned with X-ray fluorescence spectrometer, is surveyed
The content of fixed wherein chemical composition.
In a preferred embodiment, method of the invention mainly includes (a) establishing standard working curve and (b) is surveyed
Al in fixed aluminium hydroxide sample to be measured2O3、Fe2O3、SiO2And Na2The content of O.
Preferably, (a) establishes standard working curve, including：
1) multiple aluminium hydroxide standard samples are provided, Al in each standard sample2O3、Fe2O3、SiO2And Na2Quality shared by O
Than different；
That is, in selection standard sample, need to be selected according to each element different content level in aluminium hydroxide to establish song
Standard sample at least four of line；
It should be noted that the quantity of aluminium hydroxide standard sample is not particularly restricted, those skilled in the art can be with
It is selected according to actual needs, a specific embodiment according to the present invention, the quantity of aluminium hydroxide standard sample can not
Less than 4.Inventor has found, when the quantity of aluminium hydroxide standard sample is no less than 4, can better meet subsequent standards
The required precision of working curve, so that provided by the invention wait for test sample based on x-ray fluorescence spectrometry aluminium hydroxide
The definite value error smaller that numerical value in product obtained by each component content is obtained with chemical method.
Such as can be, according to the content of routine testing sample, to select a series of suitable standard specimens, selected series mark
Quasi- sample is as shown in table 1.
1 standard sample of table
2) buck：5-10 grams of aluminium hydroxide standard sample is weighed in each sample in mortar, continuously grinding 15
~35min, such as can be grinding 15min, 20min, 25min, 30min or 35min, sample granularity reaches≤200 mesh, such as
Can be 200 mesh of granularity, 180 mesh, 160 mesh, 150 mesh, 120 mesh, 100 mesh, 90 mesh, 80 mesh, 60 mesh, 50 mesh or 40 mesh etc., it is excellent
80~150 mesh are selected as, ensures that sample is uniform, meets fluorescent powder tabletting requirement.
It should be noted that the present invention is added without any auxiliary agent in process of lapping.Bonding not only can be reduced
The environmental pollution that agent or other auxiliary agents etc. are brought can also further decrease testing cost, promote detection speed.
3) pressed powder：Standard sample is carried out by pressed powder using pressure-like machine, standard sample tabletting is made；Specific packet
It includes：Pressure-like pallet is cleaned, plastic hoop inner wall, outer wall, two sections are placed on 1/100 balance, are reset, disposable to weigh 5 grams
Sample after grinding flattens, pressure-like machine pressure-like, 30~50MPa of pressure, 20~40s of static pressure, keeps sample surface smooth, granularity is equal
It is even, plastic hoop edge residual powder is cleaned, sample mark is for use.It is spare to clean mortar.Typical but unrestricted, pressure can be
30MPa, 35MPa, 40MPa, 45MPa or 50MPa, static pressure 20s, 25s, 30s, 35s or 40s.
It should be noted that the present invention does not do specifically limited, ability for the concrete operations parameter during pressed powder
Field technique personnel can be adjusted according to actual conditions, as long as obtained tabletting meets subsequent Xray fluorescence spectrometer
Analysis measures.The pressed powder can on the special pressure-like machine of outfit normal-temperature operation, step is simple, and speed is fast, is easy to
Operation.
4) fluorescence analysis：The emissive porwer of each ingredient in bioassay standard sample tabletting is distinguished using Xray fluorescence spectrometer；
Present invention determine that the thinking of optimum analysis condition includes：The selection chemical composition sample close with test sample is waited for is swept
It retouches, is typically chosen 1,2 lines of K α as analysis spectral line, maximum peak position is actually detected peak position；Analyzing crystal is typically chosen principle
It is the most elements that LiF is suitble within the scope of Ni~Te, PET is suitable for the element within the scope of Al~Cl；Light pipe voltage, electric current,
The factors such as collimator will consider, and keep fluorescence intensity to be in instrument optimum resolution range as possible；PHD (pulse heights point
Cloth) window analysis increases window as far as possible；Background is typically chosen at 2 points and is used as background, when characteristic signal intensity is higher than background signal
At 10 times or more, background intensity can be ignored, to shorten sweep time；Analysis time is when scanning signal deviation is less than 0.3%
As the optimized analysis time.
The optimum analysis condition that the present invention finally determines is as shown in table 2.
2 analysis condition of table
5) using a series of reflected intensity of each ingredient obtained to inner quality standard sample measurements, in conjunction with each ingredient in sample
In mass percentage, by x-ray fluorescence characteristic spectral line intensity and corresponding Al2O3、Fe2O3、SiO2And Na2O mass hundred
Divide content to carry out linear regression, respectively obtains Al2O3、Fe2O3、SiO2And Na2O corresponds to the mark of x-ray fluorescence characteristic spectral line intensity
Quasi- working curve.Using mass percentage as abscissa, it is the working curve that ordinate draws each ingredient that XRF, which measures intensity,.
In institute's mark sample, relevant parameter such as 3 institute of table of each ingredient percentage composition standard working curve associated with intensity
Show.
3 working curve of table
| Project | Intercept | Slope | SEE |
| Al2O3 | 34.73322 | 0.04502 | 0.017820 |
| Fe2O3 | 0.00130 | 0.01348 | 0.000776 |
| SiO2 | -0.00352 | 0.10941 | 0.003793 |
| Na2O | -0.05169 | 0.10891 | 0.103756 |
The relevant parameter of the regression equation for each ingredient that table 3 obtains can be incorporated into x-ray fluorescence by computer software
In the control program of spectrometer.
Preferably, the Al in aluminium hydroxide sample to be measured (b) is measured2O3、Fe2O3、SiO2And Na2The content of O, including：
1) buck；
2) pressed powder；
The concrete operations mode and operating parameter of buck and pressed powder during this and above-mentioned standard work are bent
Buck during the foundation of line is identical with operating parameter with the concrete operations mode of pressed powder, and details are not described herein；
3) Xray fluorescence spectrometer is used to measure the emissive porwer of each ingredient in aluminium hydroxide print to be measured；Fluorescence spectrum
The quality of each ingredient in aluminium hydroxide print to be measured can be calculated in control program in instrument automatically according to the relevant parameter in table 3
Percentage composition；
The analysis condition of Xray fluorescence spectrometer during this and point during the foundation of above-mentioned standard working curve
Analysis condition is identical, and details are not described herein.
In a specific embodiment, the method institute of component content in aluminium hydroxide is measured using the method for the present invention
The equipment used for example can be for：
Wavelength dispersion type x ray fluorescence spectrum analyzer；Detector is gas proportional counter and scintillation counter；It is maximum
Power 3.6kW；
ZHY-401A pressure-like machines；And the agate mortar of Ф 12cm.
To analyze the accuracy that method through the invention measures the content of each ingredient in print, the present invention is according to loading
Product preparation method and analysis condition analyze existing sample, and standard value, the standard chemical method provided with commercial product
Testing result compares, and analysis data result is shown in Table 4.
4 accuracy analysis result of table
The precision that result is measured to method therefor of the present invention is tested, and an aluminium hydroxide sample is taken, according to above-mentioned examination
Sample is ground and pressed powder method prepares 10 prints respectively, and using Xray fluorescence spectrometer, condition is distinguished according to the above analysis
Each print is measured, measurement result is shown in Table 5.
5 precision test result of table
| Detection project | Al2O3 | Fe2O3 | SiO2 | Na2O |
| Print 1 | 64.63 | 0.0096 | 0.010 | 0.15 |
| Print 2 | 64.47 | 0.0090 | 0.011 | 0.13 |
| Print 3 | 64.75 | 0.0087 | 0.011 | 0.12 |
| Print 4 | 64.76 | 0.0088 | 0.010 | 0.14 |
| Print 5 | 64.59 | 0.0095 | 0.012 | 0.16 |
| Print 6 | 64.81 | 0.0089 | 0.010 | 0.13 |
| Print 7 | 64.57 | 0.0091 | 0.010 | 0.12 |
| Print 8 | 64.51 | 0.0094 | 0.011 | 0.13 |
| Print 9 | 64.43 | 0.0091 | 0.012 | 0.14 |
| Print 10 | 64.49 | 0.0093 | 0.009 | 0.11 |
| Average value | 64.60 | 0.00914 | 0.0106 | 0.133 |
| SD | 0.133 | 0.000 | 0.001 | 0.015 |
| RSD | 0.002 | 0.033 | 0.091 | 0.112 |
Wherein, SD indicates that standard deviation, RSD indicate relative standard deviation, and the numerical value of the two is in reasonable range, originally
The detection accuracy of the method for invention is high.
By the correction data of table 4 and table 5 it is found that the x ray fluorescence spectrometry of the present invention analyzes ingredient in aluminium hydroxide
The accuracy of the method for content and precision are high, and repeatability and reproducibility is better than standard chemical method, can substitute completely existing
Standard chemical method in technology measures aluminium hydroxide.The method of the present invention is easy to operate simultaneously, and analysis time is short, and no chemistry is dirty
Dye, it is at low cost.
Second aspect provides a kind of by above-mentioned x ray fluorescence spectrometry analysis hydrogen-oxygen at least one embodiment
Change the aluminium hydroxide obtained after the method analysis of component content in aluminium.
The third aspect provides a kind of aluminium hydroxide as production float glass at least one embodiment
Application in raw material.
The second aspect of the present invention and the third aspect are analyzed ingredient in aluminium hydroxide with x ray fluorescence spectrometry above-mentioned and are contained
The method of amount be based on same inventive concept, thus at least have with aforementioned X-ray fluorescent spectrometry analyze aluminium hydroxide in
The identical advantage of method of component content, details are not described herein by the present invention.
The present invention is further explained in the light of specific embodiments.
Embodiment 1-3
A kind of method that x ray fluorescence spectrometry analyzes component content in aluminium hydroxide, according to said sample grinding and powder
Last tabletting method is respectively ground 3 aluminium hydroxides (Shanghai aluminium hydroxide) sample, and pressed powder prepares sample,
It is analyzed using above-mentioned analysis condition and working curve using X-ray fluorescence spectra, the results are shown in Table 6 for data measured.
6 embodiment 1-3 test results of table
| Project | Al2O3 | Fe2O3 | SiO2 | Na2O |
| Embodiment 1 | 65.57 | 0.0085 | 0.011 | 0.12 |
| Embodiment 2 | 65.12 | 0.0048 | 0.010 | 0.31 |
| Embodiment 3 | 64.82 | 0.0092 | 0.012 | 0.14 |
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of method of component content in x ray fluorescence spectrometry analysis aluminium hydroxide, which is characterized in that including following step
Suddenly：
Grinding；
Pressed powder；
Using x ray fluorescence spectrometry, the emissive porwer of each ingredient in print is measured, it is bent using the work of established each ingredient
Line carries out Al in aluminium hydroxide print to be measured2O3、Fe2O3、SiO2And Na2The analysis of O content.
2. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 1
It is 15~35min in the time of, grinding, the mesh of the granularity of the sample ground≤200, preferably 80~150 mesh.
3. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 1
In, during pressed powder, 30~50MPa of pressure, 20~40s of static pressure.
4. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 1
In the mode for establishing the working curve of each ingredient includes：
There is provided multiple aluminium hydroxide standard samples, Al in each standard sample2O3、Fe2O3、SiO2And Na2Mass ratio shared by O is respectively not
It is identical；
Standard sample is ground respectively and pressed powder, standard sample tabletting is made；
The emissive porwer of each ingredient in bioassay standard sample tabletting is distinguished using Xray fluorescence spectrometer；
By x-ray fluorescence characteristic spectral line intensity and corresponding Al2O3、Fe2O3、SiO2And Na2O mass percentages carry out linear
It returns, respectively obtains Al2O3、Fe2O3、SiO2And Na2O corresponds to the standard working curve of x-ray fluorescence characteristic spectral line intensity.
5. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 4
In the quantity of standard sample is >=4.
6. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 4
It is 15~35min in the time of, grinding, the mesh of the granularity of the sample ground≤200, preferably 80~150 mesh；
And/or during pressed powder, 30~50MPa of pressure, 20~40s of static pressure.
7. analyzing the side of component content in aluminium hydroxide according to claim 1~6 any one of them x ray fluorescence spectrometry
Method, which is characterized in that be respectively using the determination condition of each ingredient in Xray fluorescence spectrometer measurement aluminium hydroxide to print：
Al2O3：2 θ 144.65, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal PET, collimator 0.25,
PHD40~100, interference element is without sweep time 20s；
Fe2O3：2 θ 57.53, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal LiF200, collimator 0.15,
PHD40~100, interference element is without sweep time 20s；
SiO2：2 θ 109.001, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal PET, collimator 0.60,
PHD50~95, interference element is without sweep time 12s；
Na2O：2 θ 23.951, wavelengthVoltage 30kV, electric current 80mA, analyzing crystal AX06, collimator 0.60,
PHD40~100, interference element is without sweep time 20s.
8. the method for component content, feature exist in x ray fluorescence spectrometry analysis aluminium hydroxide according to claim 7
In the print includes aluminium hydroxide print and standard sample print to be measured.
9. by the method for component content in claim 1~8 any one of them x ray fluorescence spectrometry analysis aluminium hydroxide
The aluminium hydroxide obtained after analysis.
10. application of the aluminium hydroxide in the raw material as production float glass described in claim 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810604889.2A CN108802084A (en) | 2018-06-12 | 2018-06-12 | X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide |
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| CN114460117A (en) * | 2022-03-16 | 2022-05-10 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
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| CN111855719A (en) * | 2020-07-29 | 2020-10-30 | 河北南玻玻璃有限公司 | Sample preparation method for analyzing chemical components of quartz sandstone by X-ray fluorescence spectrometry |
| CN112129798A (en) * | 2020-10-21 | 2020-12-25 | 中国食品药品检定研究院 | Method for measuring content of native copper in Chinese patent medicine |
| CN113075148A (en) * | 2021-03-22 | 2021-07-06 | 久泰能源(准格尔)有限公司 | Method for measuring carbon content on surface of catalyst in MTO (methanol to olefin) process |
| CN113075148B (en) * | 2021-03-22 | 2023-06-16 | 久泰能源(准格尔)有限公司 | Method for measuring carbon content of catalyst surface in MTO process |
| CN113237907A (en) * | 2021-04-08 | 2021-08-10 | 中国铝业股份有限公司 | Method for measuring fluorine content in fluorine-carrying alumina by X-ray fluorescence spectrometry |
| CN114460117A (en) * | 2022-03-16 | 2022-05-10 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
| CN114460117B (en) * | 2022-03-16 | 2023-06-06 | 清远南玻节能新材料有限公司 | Method for detecting component content of aluminum hydroxide product |
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