CN102809578A - Method of measuring component contents in fluorite by applying X fluorescence powder tablet pressing method - Google Patents
Method of measuring component contents in fluorite by applying X fluorescence powder tablet pressing method Download PDFInfo
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Abstract
The invention discloses a method of measuring component contents in fluorite by applying an X fluorescence powder tablet pressing method. The method comprises the following steps of: (1) pressing a fluorite standard sample and an adhesive into a group of standard sample pressed tablets with proper CaF2 gradient contents; (2) preparing a sample to be tested and the adhesive into a sample pressed tablet to be tested; (3) analyzing the standard sample pressed tablet by using an X fluorescence spectrometer and acquiring a linear regression analysis curve by enhancing absorption and deducting spectral line overlapping interference after the analysis is finished, then selecting and using the working curve to measure the sample pressed tablet to be tested, and calculating the contents of various components of the fluorite according to correspondence of analyzed spectral line intensity and concentration; and (4) pressing the standard sample pressed tablet and the sample pressed tablet to be tested by uniformly mixing and grinding the fluorite standard sample as well as the fluorite sample to be tested and the adhesive respectively, sieving through a 300-mesh screen and finally pressing into tablets in a tablet press. The method is quick and accurate, the check cost is reduced, and the check efficiency is greatly increased.
Description
Technical field
The present invention relates to a kind of method of measuring component concentration in the fluorite, especially a kind of method of using component concentration in the X fluorescent powder pressed disc method mensuration fluorite.
Background technology
Fluorite is claimed fluorite again, in steel and iron industry, is mainly used in slag making in blast furnace or the pneumatic steelmaking, and fluorite is a kind of typical silicate mineral, and its principal ingredient is calcium fluoride, silicon dioxide and a spot of carbonate, phosphate.The important evidence of estimating its quality index is components contents such as calcium fluoride, silicon dioxide.At present, each component generally adopts chemical method and fluorescence method in the mensuration fluorite, and the chemical method analysis operation is loaded down with trivial details, and wherein the calcium fluoride Determination on content will approximately need six hours through twice filtration.Fluorescence method adopts the fusion sample preparation more, for example the 26th volume the 5th phase 419-420 page or leaf " calcium fluoride in the x-ray fluorescence spectrometry fluorite " of distribution " test of rock ore deposit " in October, 2007.Adopt X fluorescence fusion method to exist the specimen preparation cycle long, the not wield shortcoming of analysis operation.
Summary of the invention
The technical matters that the present invention will solve provides the method that a kind of analysis speed application X fluorescent powder pressed disc method fast, easy and simple to handle is measured component concentration in the fluorite.
For solving the problems of the technologies described above, method step of the present invention is:
(1) is pressed into one group with fluorite standard model and cementing agent suitable CaF is arranged
2The standard model compressing tablet of gradient content;
(2) testing sample and cementing agent are pressed into the testing sample compressing tablet;
(3) utilize X XRF analytical standard sample compressing tablet, through behind the deduction that strengthens absorption and overlap of spectral lines interference, obtain the linear regression analysis curve after analysis finishes; Select for use this working curve to carry out the mensuration of testing sample compressing tablet then,, calculate the content of fluorite various ingredients according to the corresponding relation of analysis spectral line intensity and concentration;
(4) above-mentioned drawing method with standard model compressing tablet and testing sample compressing tablet is: fluorite standard model and fluorite sample to be measured mix the back with cementing agent respectively and grind, and cross 300 mesh sieves then, difference tablet forming appearance in the last sheeter.
In the step according to the invention (4), said sheeter pressure 15MPa, voltage stabilizing time 15s.Said standard model and testing sample mix according to mass ratio 1:4～1:7 with cementing agent respectively, and said cementing agent is lithium carbonate, lithium tetraborate, lithium metaborate and/or starch.Said standard model and testing sample preferably mix according to mass ratio 1:5 with cementing agent respectively, and cementing agent is preferably lithium tetraborate and the lithium metaborate hybrid adhesive by weight 67:33.Standard model and testing sample are preferably in cementing agent respectively and grind 60s in the vibromill.
In the step according to the invention (3); When utilizing the X XRF to analyze, the analysis spectral line of calcium, fluorine, silicon, phosphorus, sulphur, iron, potassium and eight kinds of elements of sodium, crystal, detector, spectrum peak 2 θ angles and Measuring Time are respectively: aluminium Ca-Ka, LiF1, PC, 113.118 °, 20s; Fluorine F-Ka, R * 25, PC, 75.952 °, 40s; Silicon Si-Ka, PET, PC, 109.036 °, 20s; Phosphorus P-Ka, Ge, PC, 141.078 °, 60s; Sulphur S-Ka, Ge, PC, 110.712 °, 20s; Iron Fe-Ka, LiF1, SC, 57.500 °, 10s; Potassium K-Ka, LiF1, PC, 136.686 °, 20s; Sodium Na-Ka, R * 25, PC, 47.030 °, 60s; Set analysis condition: light pipe voltage 50KV, electric current 60mA, optical filter does not have, and attenuator does not have.
In the step according to the invention (1): select for use 5 kinds of fluorite standard models to be pressed into the standard model compressing tablet with cementing agent respectively earlier, CaF in the fluorite standard model of selecting for use
2Mass percent be respectively: 94.813%, 92.475%, 65.733%, 76.709%, 93.185%; Again with CaF in the fluorite standard model
2Content be 65.733% and 93.185% two kind of fluorite standard model to be mixed into mass percent by weight 1:1 be 79.459% hybrid standard sample, be pressed into the standard model compressing tablet with cementing agent then; Thereby obtain one group suitable CaF is arranged
2The standard model compressing tablet of gradient content.
Adopt the beneficial effect that technique scheme produced to be: this method is innovated specimen preparation and analytical instrument etc. on the basis that takes into full account fluorescence method analysis advantage.The grain effect that powder pressing method produces adds measures such as cementing agent and abundant stirring and evenly mixing and obtains fine solution through taking 300 mesh.
The present invention adopt to survey fluorine element to X fluorometric assay calcium fluoride and the problem that light element is difficult to measure, fluorescent yield is low occurs, this method through improve voltage strength, reduce dilution ratio, utilize special-purpose RX * measures such as 25 crystal make the low problem of fluorine element line strength obtain fine solution.
This method has solved CaF in the fluorite
2Assay can't adopt powder pressing method and pass through to measure F element conversion CaF
2A difficult problem; The content of various ingredients in can the rapid and accurate determination fluorite, method has quick and precisely not only been simplified numerous and diverse formality of X fluorescence spectrum method for measuring fluorite; Reduce inspection cost; And improved checkability greatly, can let factory in time grasp the fluorite main chemical compositions, thereby better control production technology.This method makes full use of existing instrument and equipment, is equipped with succinctly easily that pressed-disc technique can realize, have easy and simple to handle, be easy to grasp, accuracy and the good characteristics of repeatability.Through a large amount of experimental data checkings, the present invention can satisfy production technology and analytic approach error requirements, especially analysis time are effectively shortened, and is easy and simple to handle, is easy to grasp, and analytical precision and accuracy can satisfy production, scientific research needs.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
Should be to utilize the wavelength dispersion X-fluorescence appearance to measure with the method for component concentration in the X fluorescent powder pressed disc method mensuration fluorite, concrete steps be described below:
1, selects all higher spectral line of intensity and signal-to-background ratio as analytic curve; The analysis spectral line of calcium, fluorine, silicon, phosphorus, sulphur, iron, potassium and eight kinds of elements of sodium, crystal, detector, spectrum peak 2 θ angles and Measuring Time are respectively: 113.118 ° of 20s of aluminium Ca-Ka LiF1 PC, fluorine F-Ka R * 75.952 ° of 40s of 25 PC, 109.036 ° of 20s of silicon Si-Ka PET PC, 141.078 ° of 60s of phosphorus P-Ka Ge PC, 110.712 ° of 20s of sulphur S-Ka Ge PC, 57.500 ° of 10s of iron Fe-Ka LiF1 SC, 136.686 ° of 20s of potassium K-Ka LiF1 PC, sodium Na-Ka R * 47.030 ° of 60s of 25 PC; Set analysis condition: light pipe voltage 50KV, electric current 60mA; Optical filter does not have, and attenuator does not have.
2, preparation has suitable CaF for one group
2The standard model compressing tablet of gradient content and testing sample compressing tablet preferably adopt following method preparation standard sample compressing tablet: select for use 5 kinds of fluorite standard models to be pressed into the standard model compressing tablet with cementing agent respectively earlier, CaF in the fluorite standard model of selecting for use
2Mass percent be respectively: 94.813%, 92.475%, 65.733%, 76.709%, 93.185%, CaF in the fluorite standard model
2Content is according to CaF by F content in the fluorite standard certificate
2%=2.053 * F% converts and gets; Again with CaF in the fluorite standard model
2Content be 65.733% and 93.185% two kind of fluorite standard model to be mixed into the moderate mass percent of content by weight 1:1 be 79.459% hybrid standard sample; Its mixing means are pressed into the standard model compressing tablet with cementing agent then for accurately in Doppler's mixing appearance, fully mixing after the weighing in proportion; Thereby obtain one group suitable CaF is arranged
2The standard model compressing tablet of gradient content.Because composition is single in the fluorite, bad adhesion between particle, directly compacting is difficult to obtain the desirable print of intensity (sample compressing tablet), therefore needs to adopt suitable cementing agent to meet the requirements of analytic sample to obtain intensity.Compacting sample cementing agent commonly used has lithium carbonate, lithium tetraborate, lithium metaborate, starch in this method.Starch has been found following problem in practice process: because the hydroscopicity of starch is stronger, if it is not dried, the water cut of gained print is bigger; And the used PrimusII XRF of science of this method needs vacuumize separately injection port, and moisture vacuumizes and can encounter difficulties more for a long time in the print, can cause sample injection time long even can't sample introduction; And if starch is dried, its cohesiveness can reduce greatly, and crackle possibly occur after the compacting after the sample mixed and maybe can't be pressed into print.Though can obtain comparatively the desirable print of intensity but analyze carbon that interference is arranged and make cementing agent with lithium carbonate, there is not overlap of spectral lines between each component to be measured in element such as lithium, oxygen and the fluorite in lithium tetraborate, the lithium metaborate, absorption enhancement effect is also not remarkable; Therefore, lithium tetraborate, lithium metaborate are preferable cementing agent, and the employed cementing agent of this method is preferably the potpourri (mass ratio 67:33) of lithium tetraborate+lithium metaborate.For confirming the The Best Mixed ratio of sample and cementing agent, suppressed a series of prints according to different mixing ratios, its intensity is observed visible, when lithium tetraborate, lithium metaborate proportion were low, print intensity was low, phenomenon such as be prone to crackle, loosen; After the two ratio reached 1:5, print intensity was just more satisfactory, occupied high level for making in the print component to be measured as far as possible, confirmed that the cementing agent blending ratio is m
Fluorite: m
Lithium tetraborate+lithium metaborate (67:33)=1:4～1:7 is preferably 1:5.When the compacting print, whether mixing can directly have influence on precision of analysis for sample and cementing agent.In addition, because lithium tetraborate, lithium metaborate reagent particle are bigger, if without grinding direct tablet compressing, its granularity may impact analysis result.According to the particle size differences property of fluorite and cementing agent, this method has designed following mixed method: change in the beaker after sample and cementing agent are weighed up in proportion, stir until mixing with spoon, be viewed as all of the same colour on the color and luster; Pour a little mixed-powder into carry out mill in the vibrations mill mill cleaning and (select the chromium steel mill for use; Use alcohol wash in case of necessity); After work to be cleaned is accomplished, remaining mixed-powder poured in the lump pulverize 60s in the mill, collect subsequent use after 300 orders sieve.Pressure is too low or the dwell time is not enough when carrying out the compressing tablet sample preparation; The capital impacts the physical strength of print, and pressure will increase the load of hydropress more greatly, and the corresponding sample physical strength that suppresses will be big more; But in practical operation, the appearance ring damages probability by pressure to be increased.Fluorescence analysis has certain smooth finish and certain intensity is arranged with the sample requirement surface.For guaranteeing print intensity, select pressure 15Mpa for use, voltage stabilizing time 15s.Therefore adopt following method preparation standard sample compressing tablet and testing sample compressing tablet: fluorite standard model and testing sample is even according to the 1:5 mixed with cementing agent respectively; Condition pressed in sheeter pressure 15MPa, voltage stabilizing time 15 is in blocks, with the pressurized air air gun blow away be put in the exsiccator behind the surface impurity subsequent use.
3, utilize the X XRF; Create analytical approach; Suitable analysis condition is set and optimizes measuring condition well, analysis fluorite standard model compressing tablet and hybrid standard sample compressing tablet are behind the deduction through do enhancing absorption and overlap of spectral lines interference after analysis finishes; The linear regression analysis curve, related coefficient is desirable; Select for use this working curve to carry out the mensuration of fluorite sample to be tested compressing tablet then,, can calculate the content of various ingredients in the fluorite according to the corresponding relation of analysis spectral line intensity and concentration.
Precision test and accuracy test:, done a series of precision tests, accuracy test under these conditions in order to verify the feasibility of this method.Calculating mean value and relative standard deviation are analyzed 10 times in the precision test continuously to same fluorite sample; Accuracy test is chosen some fluorite samples, measures with this method, and gained result and chemical method are compared, and test figure is seen table 1, table 2.
Table 1: the precision test (n=10, w/%)
Show that through above test figure (table 1, table 2) this method utilizes x-ray fluorescence method to analyze the precision of fluorite, the production Technology requirement that accuracy can be satisfied fluorite.Compare with chemical method, this method has shortened the analytical cycle of sample greatly, have easy and simple to handle, be easy to advantages such as grasp.This method has not only been simplified numerous and diverse formality of X fluorescence spectrum method for measuring fluorite, reduces inspection cost, and has improved checkability greatly, can let factory in time grasp the fluorite main chemical compositions, thereby better control production technology.
Embodiment: should be described below with the step of the method for component concentration in the X fluorescent powder pressed disc method mensuration fluorite.
1, utilize the X XRF to create analytical approach: select analysis spectral line, crystal, detector, spectrum peak 2 θ angles and the Measuring Time etc. of calcium, fluorine, silicon, phosphorus, sulphur, iron, potassium and eight kinds of elements of sodium to analyze parameter, as shown in table 3.
2, preparation standard sample compressing tablet: select suitable standard fluorite sample, typical component content is as shown in table 4; Conduct replenishes after having selected for use certain concentration gradients, representational free fluorite sample to analyze definite value with chemical method and ICP-OES method simultaneously, and the part component concentration is as shown in table 5, obtains the fluorite standard model.Accurately take by weighing this fluorite standard model and cementing agent and in vibromill, grind 60s according to the ratio of 1:5; After 300 mesh sieves pass through; Press down appearance in blocks with the condition of sheeter 15MPa, voltage stabilizing time 15s, with the pressurized air air gun blow away be put in the exsiccator behind the surface impurity subsequent use.Promptly get the standard model compressing tablet, be put in the exsiccator subsequent use.
3, prepare hybrid standard sample compressing tablet: the part component concentrations contains the middle high-load standard model that adds these components of method making of a spot of other fluorite standard model in the fluorite standard model, accurately in Doppler's mixing appearance, fully in exsiccator, is used as the hybrid standard sample after the mixing after the weighing in proportion; The preparation method of hybrid standard sample compressing tablet is with the preparation method of standard model compressing tablet.Each component concentration is as shown in table 6.
4, the testing sample compressing tablet of preparation fluorite sample: with fluorite sample and cementing agent proportionally 1:5 mix; Condition pressed in sheeter pressure 15MPa, voltage stabilizing time 15s is in blocks; After blowing away surface impurity with the pressurized air air gun, be put in the exsiccator for use;
5, various ingredients Determination on content in the fluorite: utilize the X XRF; Create analytical approach; Analysis condition and measuring condition are set, standard model compressing tablet and hybrid standard sample compressing tablet, analysis finishes behind the deduction of back through enhancing absorption and overlap of spectral lines interference; The linear regression analysis curve, each element is linear good; Select for use this working curve to carry out the mensuration of testing sample compressing tablet then,, calculate the content of various ingredients in the fluorite according to the corresponding relation of analysis spectral line intensity and concentration.
Claims (7)
1. use the method that X fluorescent powder pressed disc method is measured component concentration in the fluorite for one kind, it is characterized in that this method step is: (1) is pressed into one group with fluorite standard model and cementing agent has suitable CaF
2The standard model compressing tablet of gradient content;
(2) testing sample and cementing agent are pressed into the testing sample compressing tablet;
(3) utilize X XRF analytical standard sample compressing tablet, through behind the deduction that strengthens absorption and overlap of spectral lines interference, obtain the linear regression analysis curve after analysis finishes; Select for use this working curve to carry out the mensuration of testing sample compressing tablet then,, calculate the content of fluorite various ingredients according to the corresponding relation of analysis spectral line intensity and concentration;
(4) above-mentioned drawing method with standard model compressing tablet and testing sample compressing tablet is: fluorite standard model and fluorite sample to be measured mix the back with cementing agent respectively and grind, and cross 300 mesh sieves then, difference tablet forming appearance in the last sheeter.
2. application X fluorescent powder pressed disc method according to claim 1 is measured the method for component concentration in the fluorite, it is characterized in that: in the said step (4), and said sheeter pressure 15MPa, voltage stabilizing time 15s.
3. application X fluorescent powder pressed disc method according to claim 1 is measured the method for component concentration in the fluorite; It is characterized in that: in the said step (4); Said standard model and testing sample mix according to mass ratio 1:4～1:7 with cementing agent respectively, and said cementing agent is lithium carbonate, lithium tetraborate, lithium metaborate and/or starch.
4. application X fluorescent powder pressed disc method according to claim 3 is measured the method for component concentration in the fluorite; It is characterized in that: in the said step (4); Said standard model and testing sample mix according to mass ratio 1:5 with cementing agent respectively, and cementing agent is lithium tetraborate and the lithium metaborate hybrid adhesive by weight 67:33.
5. application X fluorescent powder pressed disc method according to claim 1 is measured the method for component concentration in the fluorite, and it is characterized in that: in the said step (4), standard model and testing sample grind 60s with cementing agent respectively in vibromill.
6. use the method that X fluorescent powder pressed disc method is measured component concentration in the fluorite according to described any one of claim 1-5; It is characterized in that; In the said step (3); When utilizing the X XRF to analyze, the analysis spectral line of calcium, fluorine, silicon, phosphorus, sulphur, iron, potassium and eight kinds of elements of sodium, crystal, detector, spectrum peak 2 θ angles and Measuring Time are respectively: aluminium Ca-Ka, LiF1, PC, 113.118 °, 20s; Fluorine F-Ka, R * 25, PC, 75.952 °, 40s; Silicon Si-Ka, PET, PC, 109.036 °, 20s; Phosphorus P-Ka, Ge, PC, 141.078 °, 60s; Sulphur S-Ka, Ge, PC, 110.712 °, 20s; Iron Fe-Ka, LiF1, SC, 57.500 °, 10s; Potassium K-Ka, LiF1, PC, 136.686 °, 20s; Sodium Na-Ka, R * 25, PC, 47.030 °, 60s; Set analysis condition: light pipe voltage 50KV, electric current 60mA, optical filter does not have, and attenuator does not have.
7. use the method that X fluorescent powder pressed disc method is measured component concentration in the fluorite according to described any one of claim 1-5; It is characterized in that; In the said step (1): select for use 5 kinds of fluorite standard models to be pressed into the standard model compressing tablet with cementing agent respectively earlier, CaF in the fluorite standard model of selecting for use
2Mass percent be respectively: 94.813%, 92.475%, 65.733%, 76.709%, 93.185%; Again with CaF in the fluorite standard model
2Content be 65.733% and 93.185% two kind of fluorite standard model to be mixed into mass percent by weight 1:1 be 79.459% hybrid standard sample, be pressed into the standard model compressing tablet with cementing agent then; Thereby obtain one group suitable CaF is arranged
2The standard model compressing tablet of gradient content.
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