CN103969272A - Method and system for determination of cement components by X ray fluorescence analysis - Google Patents
Method and system for determination of cement components by X ray fluorescence analysis Download PDFInfo
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- CN103969272A CN103969272A CN201310036148.6A CN201310036148A CN103969272A CN 103969272 A CN103969272 A CN 103969272A CN 201310036148 A CN201310036148 A CN 201310036148A CN 103969272 A CN103969272 A CN 103969272A
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Abstract
The invention discloses a method and a system for determination of cement components by X ray fluorescence analysis. The method comprises the following steps of preparing a standard cement sample fuse piece and a cement sample fuse piece to be detected and measuring X fluorescence intensity, converting all detected element intensity values of the cement sample fuse piece to be detected into intensity values at a dilution ratio of 5, calculating contents of all chemical components of the cement sample fuse piece to be detected, calculating the sum of the contents of all the chemical components of the cement sample fuse piece to be detected, and determining if the difference of the sum (represented by SUM) of the contents of all the chemical components of the cement sample fuse piece to be detected and the sum (represented by SUMS) of the contents of all the chemical components of the standard cement sample fuse piece is in a preset range until after the multiple calculation processes, the difference is in the preset range, wherein the last calculated mass fraction is used as a measurement result. A data processing device of the system for determination of cement components by X ray fluorescence analysis is used for executing the above processes. The method and system have simple operation processes and are suitable for practical application.
Description
Technical field
The present invention relates to a kind of cement composition determination techniques, particularly relate to a kind of method and system that adopt x-ray fluorescence analysis to measure cement composition.
Background technology
At present, when fusion method x-ray fluorescence analysis cement sample, first to prepare serial calibration sample, calibration sample melted is prepared into bead by fixing standard dilution ratio, then make working curve by the x-ray fluorescence intensity of measuring serial calibration sample.Then the loss on ignition under melt temperature according to cement sample and flux, according to the requirement of standard dilution ratio, quantitatively take exactly sample and flux, in the inaccurate and molten sample process of any weighing, sample or the loss of flux and the temperature error of molten sample equipment and temperature non all can cause error for measurement result.Therefore, cement series calibration sample, molten sample equipment, flux loss on ignition and operating personnel's technical ability is all had higher requirements.
Because the defect that exists in above-mentioned existing x-ray fluorescence analysis, actively research and innovation in addition of the inventor, to founding a kind of method that new x-ray fluorescence analysis measures cement composition to improve above-mentioned defect.
Summary of the invention
Fundamental purpose of the present invention is, provides a kind of new x-ray fluorescence analysis to measure the method and system of cement composition, makes its operating process more simple and easy to do, thereby is suitable for practicality.
For achieving the above object, the present invention proposes a kind of method of x-ray fluorescence analysis mensuration cement composition, and it comprises:
Step 1, preparation standard cement sample fuse piece, the dilution ratio of this fuse piece is 5;
Step 2, prepares cement sample fuse piece to be measured;
Step 3, measures the intensity of each chemical composition corresponding element in above-mentioned standard cement sample fuse piece and cement sample fuse piece to be measured with x-ray fluorescence analyzer;
Step 4, it is 5 intensity level that each element-intensities cement sample to be measured being recorded according to formula (1) is converted into dilution ratio,
In formula: I
i, 5for the x-ray fluorescence intensity of chemical analysis i corresponding element in the dilution ratio cement sample fuse piece to be tested that is 5, R is the dilution ratio of cement sample fuse piece to be tested, I
ifor the x-ray fluorescence intensity of chemical analysis i corresponding element in cement sample fuse piece to be tested, α
i,ffor influence coefficient,
Calculate the content of the each chemical composition of cement sample to be measured according to formula (2),
In formula: C
ifor the massfraction of chemical analysis i in cement sample to be tested, I
i,sfor the x-ray fluorescence intensity of the accurate sample chemical composition of standard i corresponding element, C
i,sfor the massfraction of chemical analysis i in standard sample;
Calculate the content summation SUM of the each chemical composition of cement sample to be measured according to formula (3),
SUM=∑C
i(3)；
Step 5, gives R assignment, and calculates the massfraction C of chemical analysis i in cement sample to be tested according to step 4
iand the content summation SUM of the each chemical composition of cement sample to be measured, and whether the difference SUM-SUMS that judges the content summation SUMS of each chemical composition in the content summation SUM of the each chemical composition of cement sample to be measured and standard model is in preset range;
If so, the massfraction C of chemical analysis i in the above-mentioned cement sample to be tested calculating
ibe measurement result;
If not, perform step 6;
Step 6, repeating step 5, wherein gives R assignment again, in the time that the difference of the content summation SUMS of each chemical composition in the content summation SUM of the each chemical composition of cement sample to be measured and standard model is in preset range, the massfraction C that this time calculates
ibe measurement result.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, and in described step 2, the dilution ratio of the cement sample fuse piece to be measured of preparation is 2.5-10.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, and in described step 5, giving R assignment is for the first time 5.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, and described preset range is-0.05%-0.05%.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, in the time of SUM>SUMS, is less than last time R value again in step 6 R assignment, in the time of SUM<SUMS, is greater than last time R value again in step 6 R assignment.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, and in step 6, again giving the scope of the step-length of R assignment is 0.001-0.1.
For achieving the above object, the present invention also proposes a kind of X-ray fluorescence analyzing system, and it comprises data processing equipment, and described data processing equipment is carried out aforesaid x-ray fluorescence analysis and measured step 4 in the method for cement composition to step 6.
By technique scheme, the method and system of cement composition are measured in the x-ray fluorescence analysis that the embodiment of the present invention provides, in the time preparing sample to be tested fuse piece, without sample and flux are weighed, melt temperature and time are also without strict demand, after only need getting a strockle flux and little scoop sample product and being put into and mixing in the crucible that molten sample uses, under the arbitrary temp between 950 DEG C～1200 DEG C, melt to the clarification of range estimation melt and can be made into bead; Make when working curve also without adopting the special series standard sample of XRF analysis, of can the finish the work making of curve of a common cement standard sample.Thereby reduce Operating Complexity and the high request to performance accuracy, made test job simple.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of instructions, below is described in detail as follows with preferred embodiment of the present invention.
Brief description of the drawings
Fig. 1 is the computation process process flow diagram that the present invention proposes method one embodiment of x-ray fluorescence analysis mensuration cement composition.
Embodiment
Technological means and effect of taking for reaching predetermined goal of the invention for further setting forth the present invention, below in conjunction with preferred embodiment, its embodiment of method and system of the x-ray fluorescence analysis proposing according to the present invention being measured to cement composition is described in detail as follows.
The preparation method of fuse piece
1, standard model fuse piece preparation
The preparation dilution ratio standard cement sample fuse piece that is 5, has accurately taken card ms gram, sample of cement standard (calcination base), and 5ms gram of flux (calcination base) puts into Pt95-Au5 crucible, the sample in crucible and flux is carefully uniformly mixed with glass bar.In high temperature furnace more than 950 DEG C, melting more than 5 minutes melts completely to sample, pours into and is preheating in 900 DEG C of above Pt95-Au5 molds, is chilled to after room temperature, takes off in exsiccator and preserves.
Cement sample fuse piece preparation to be measured
Get little spoon cement sample to be measured and (do not differ from 1 times with the amount of taking of standard model, available other estimated utensil and estimated as counter balance) and a strockle flux (do not differ from 1 gram with the amount of taking of standard model, available other estimated utensil and estimated as counter balance), melting slab, without the strict temperature and time of controlling fuse piece, evenly clarify and be as the criterion to estimate melt; Water content in flux is not done to requirement yet.
2, the measurement of each chemical analysis x-ray fluorescence intensity in fuse piece
By the intensity of whole chemical analysis corresponding elements in x-ray fluorescence analyzer measurement standard sample and two fuse pieces of cement sample to be measured, as the intensity of calcium oxide measurement calcium constituent, silicon dioxide is measured the intensity of element silicon, in general cement sample, need the x-ray fluorescence intensity of silicon, iron, aluminium, calcium, magnesium, potassium, sodium, sulphur, titanium, phosphorus and 11 elements of manganese to measure minimum will measurement silicon, iron, aluminium, calcium, magnesium, potassium and seven elements of sulphur.
3, the calculating of cement sample chemical analysis to be measured
Determine a series of dilution ratio R of sample fuse piece with method of trials and errors, so each element-intensities of sample is converted into dilution ratio is 5 intensity level I for back-pushed-type (1) or other valid formula
i, 5.
Calculate the content of each chemical analysis in sample by formula (2), with each chemical analysis sum SUM in formula (3) calculating sample.When each chemical analysis sum in sample equates with each chemical analysis sum SUMS in standard model or in preset range time, the result of corresponding each chemical analysis is the measurement result of corresponding chemical analysis in sample.
SUM=∑C
i(3)
In formula: I
i, 5for the x-ray fluorescence intensity of i chemical analysis corresponding element in the dilution ratio cement sample fuse piece to be measured that is 5;
R is the dilution ratio of cement sample fuse piece to be measured;
I
ifor the x-ray fluorescence intensity of i chemical analysis corresponding element in cement sample fuse piece to be measured;
C
ifor the massfraction of chemical analysis i in cement sample to be measured;
I
i, sfor the x-ray fluorescence intensity of the dilution ratio accurate sample i of the standard chemical analysis corresponding element that is 5;
C
i, sfor the massfraction of chemical analysis i in the accurate sample of standard;
α
i, ffor influence coefficient, can adopt method of the prior art to obtain, also can adopt application number is that the method for introducing in 2012105744112 patent documentations is measured.For ensureing the fully open of present techniques scheme, the assay method of describing influence coefficient at this is as follows.
Select the daily comparison test sample of national cement Product Quality Verification Centers, cement type is that the portland cement of PI type is tested sample, selects lithium tetraborate as flux, the bead of 15 different dilution ratio R ' of preparation.Adopt RIGAKU ZSX Primus II x-ray fluorescence analyzer (end window Rh target X-ray tube) to carry out x-ray fluorescence intensity mensuration to each bead, obtain the X ray intensity I of each composition in each sample '.If each constituent concentration C '
ibe 100, and I ' and R ' * I ' carried out to initial point and do linear regression analysis and obtain K
2and K
1, can try to achieve the corresponding slope of R ' * I ' is K
2with the corresponding slope K of I
1, according to formula α
i, f=K
2/ K
1obtain the flux influence coefficient α of each element
i, f.
Example 1
Chemical analysis with " French cement " for calibration sample mensuration cement sample
France's cement refers to 2011 annual French cement International Comparison samples, standard specimen concentration in its chemical group prejudice table 1.Operating process is as follows:
1, by French cement 950 degrees Celsius of lower calcinations more than 60 minutes, take out and in exsiccator, be cooled to room temperature, then accurately taking 1.2000 grams puts into Pt95-Au5 crucible with 6.0000 grams of sodium tetraborate flux and mixes, melting 15 minutes in the high temperature furnace of 950 DEG C, pour into and be preheating in 900 DEG C of above Pt95-Au5 molds, be chilled to after room temperature, take off bead and preserve in exsiccator.
2, get approximately 1.2 grams of cement sample to be measured and 6 grams of flux, in high temperature furnace, melt to after the even clarification of melt, pour into and be preheating in 900 DEG C of above Pt95-Au5 molds, be chilled to after room temperature, take off bead and preserve in exsiccator.
3, the ray fluorescence intensity of each chemical analysis in difference Measurement and calibration sample and cement sample to be measured, the results are shown in Table standard specimen intensity and sample intensity in 1.Be that the dilution ratio correction coefficient measurement result providing in 2012105744112 patent documentations is also listed in table 1 by application number.
4, according to flow process shown in Fig. 1.Make R=5, with formula (1), formula (2) and formula (3) are calculated respectively I
i, 5, C
iwith SUM(i=silicon, iron, aluminium, calcium, magnesium, potassium, sulphur and titanium or its oxide), the results are shown in Table the row at sequence number 1 place in 2.Because SUM value is 106.45, be greater than the summation 99.20 of standard model, therefore make R value reduce 0.1, i.e. R=4.9, repeats I
i, 5, Ci and SUM calculate, and the results are shown in Table the row at sequence number 2 places in 2.So repay while trying to be calculated to R=4.5, SUM value is 98.90, is less than the summation 99.20 of standard model.And then R value is added to 0.01, even R=4.51 repeats I
i, 5, C
icalculate with SUM, so repay examination and be calculated to the summation 99.20 that SUM value is more than or equal to standard model.If SUM=SUMS, or SUM-SUMS≤0.05%, corresponding this sequence number R value corresponding concentration is the measurement result of each chemical analysis in sample.If SUM-SUMS > 0.05%, corresponding this sequence number R value and upper sequence number R value secondary corresponding concentration mean value is the measurement result of each chemical analysis in sample.In this example, cement sample to be measured used is the country-level standard substance GSB03201a of cement, and measurement result and standard results and error at measurment are in table 3.Table 4 is to be that 2012105744112 patent documentations are to influence coefficient measurement result reckoner according to application number.
Table 1: master data table
| Composition | Al 2O 3 | CaO | Fe 2O 3 | MgO | K 2O | SiO 2 | SO 3 | TiO 2 | SUMS |
| Standard specimen concentration | 5.14 | 61.47 | 2.52 | 5.15 | 1.00 | 20.21 | 3.45 | 0.26 | 99.20 |
| Standard specimen intensity | 20.59 | 622.71 | 75.06 | 8.81 | 24.48 | 75.60 | 31.93 | 1.20 | |
| Sample intensity | 22.02 | 695.70 | 103.03 | 2.51 | 32.94 | 85.84 | 22.52 | 1.04 | |
| α i，f | 0.065 | 0.582 | 0.866 | 0.156 | 0.403 | 0.142 | 0.332 | 0.870 |
Table 2 computational data table
| Sequence number | R | I Al2O3 | I CaO | I Fe2O3 | I MgO | I K2O | I SiO2 | I SO3 | I TiO2 |
| 1 | 5 | 22.02 | 699.70 | 103.03 | 2.51 | 32.94 | 85.84 | 22.52 | 1.04 |
| 2 | 4.9 | 21.66 | 690.23 | 102.20 | 2.46 | 32.44 | 84.45 | 22.17 | 1.03 |
| 3 | 4.8 | 21.30 | 680.77 | 101.38 | 2.42 | 31.95 | 83.06 | 21.83 | 1.02 |
| 4 | 4.7 | 20.93 | 671.30 | 100.55 | 2.38 | 31.46 | 81.67 | 21.48 | 1.01 |
| 5 | 4.6 | 20.57 | 661.84 | 99.72 | 2.34 | 30.96 | 80.28 | 21.13 | 1.01 |
| 6 | 4.5 | 20.21 | 652.37 | 98.90 | 2.29 | 30.47 | 78.88 | 20.79 | 1.00 |
| 7 | 4.51 | 20.24 | 653.32 | 98.98 | 2.30 | 30.52 | 79.02 | 20.82 | 1.00 |
| 8 | 4.52 | 20.28 | 654.27 | 99.06 | 2.30 | 30.57 | 79.16 | 20.86 | 1.00 |
| Sequence number | SUM | C Al2O3 | C CaO | C Fe2O3 | C MgO | C K2O | C SiO2 | C SO3 | C TiO2 |
| 1 | 106.45 | 5.50 | 69.07 | 3.46 | 1.47 | 1.35 | 22.94 | 2.43 | 0.22 |
| 2 | 104.94 | 5.41 | 68.14 | 3.43 | 1.44 | 1.33 | 22.57 | 2.39 | 0.22 |
| 3 | 103.43 | 5.32 | 67.20 | 3.41 | 1.42 | 1.31 | 22.20 | 2.36 | 0.22 |
| 4 | 101.92 | 5.23 | 66.27 | 3.38 | 1.39 | 1.29 | 21.83 | 2.32 | 0.22 |
| 5 | 100.41 | 5.13 | 65.33 | 3.35 | 1.37 | 1.27 | 21.46 | 2.28 | 0.22 |
| 6 | 98.90 | 5.04 | 64.40 | 3.32 | 1.34 | 1.25 | 21.08 | 2.25 | 0.22 |
| 7 | 99.05 | 5.05 | 64.49 | 3.33 | 1.34 | 1.25 | 21.12 | 2.25 | 0.22 |
| 8 | 99.20 | 5.06 | 64.59 | 3.33 | 1.35 | 1.25 | 21.16 | 2.25 | 0.22 |
Table 3: cement sample to be measured (GSB03201a cement) measurement result (%)
| Composition | C Al2O3 | C CaO | C Fe2O3 | C MgO | C K2O | C SiO2 | C SO3 | C TiO2 |
| Measured value | 5.06 | 64.59 | 3.33 | 1.35 | 1.25 | 21.16 | 2.25 | 0.22 |
| Standard value | 5.19 | 64.48 | 3.30 | 1.47 | 1.17 | 21.26 | 2.38 | 0.23 |
| Error | 0.13 | 0.11 | 0.33 | 0.12 | 0.08 | 0.10 | 0.13 | 0.01 |
Table 4: be 2012105744112 patent documentation method calculating influence coefficient α according to application number
i, freckoner
In table: y=1/ (1+R '); K=(X
tx)
-1(X
ty)
And have:
One embodiment of the present of invention also propose a kind of X-ray fluorescence analyzing system, and it is for cement sample is carried out to analytical test, and this X-ray fluorescence analyzing system comprises x-ray fluorescence intensity determinator of the prior art and data processing equipment.In the present embodiment, described data processing equipment is carried out above-mentioned x-ray fluorescence analysis and is measured step 4 in the method for cement composition to step 6.Preferably, this data processing equipment comprises the step of carrying out data processing according to the flow process shown in Fig. 1.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, although the present invention discloses as above with preferred embodiment, but not in order to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when can utilizing the technology contents of above-mentioned announcement to make a little change or being modified to the equivalent embodiment of equivalent variations, in every case be the content that does not depart from technical solution of the present invention, any simple modification of above embodiment being done according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. a method for cement composition is measured in x-ray fluorescence analysis, it is characterized in that it comprises:
Step 1, preparation standard cement sample fuse piece, the dilution ratio of this fuse piece is 5;
Step 2, prepares cement sample fuse piece to be measured;
Step 3, measures the intensity of each chemical composition corresponding element in above-mentioned standard cement sample fuse piece and cement sample fuse piece to be measured with x-ray fluorescence analyzer;
Step 4, it is 5 intensity level that each element-intensities cement sample to be measured being recorded according to formula (1) is converted into dilution ratio,
In formula: I
i, 5for the x-ray fluorescence intensity of chemical analysis i corresponding element in the dilution ratio cement sample fuse piece to be tested that is 5, R is the dilution ratio of cement sample fuse piece to be tested, I
ifor the x-ray fluorescence intensity of chemical analysis i corresponding element in cement sample fuse piece to be tested, α
i,ffor influence coefficient,
Calculate the content of the each chemical composition of cement sample to be measured according to formula (2),
In formula: C
ifor the massfraction of chemical analysis i in cement sample to be tested, I
i,sfor the x-ray fluorescence intensity of the accurate sample chemical composition of standard i corresponding element, C
i,sfor the massfraction of chemical analysis i in standard sample;
Calculate the content summation SUM of the each chemical composition of cement sample to be measured according to formula (3),
SUM=∑C
i(3)；
Step 5, gives R assignment, and calculates the massfraction C of chemical analysis i in cement sample to be tested according to step 4
iand the content summation SUM of the each chemical composition of cement sample to be measured, and whether the difference SUM-SUMS that judges the content summation SUMS of each chemical composition in the content summation SUM of the each chemical composition of cement sample to be measured and standard model is in preset range;
If so, the massfraction C of chemical analysis i in the above-mentioned cement sample to be tested calculating
ibe measurement result;
If not, perform step 6;
Step 6, repeating step 5, wherein gives R assignment again, in the time that the difference of the content summation SUMS of each chemical composition in the content summation SUM of the each chemical composition of cement sample to be measured and standard model is in preset range, the massfraction C that this time calculates
ibe measurement result.
2. the method for cement composition is measured in x-ray fluorescence analysis according to claim 1, it is characterized in that, in described step 2, the dilution ratio of the cement sample fuse piece to be measured of preparation is 2.5-10.
3. the method for cement composition is measured in x-ray fluorescence analysis according to claim 1, it is characterized in that, in described step 5, giving R assignment is for the first time 5.
4. the method for cement composition is measured in x-ray fluorescence analysis according to claim 1, it is characterized in that, described preset range is-0.05%-0.05%.
5. the method for cement composition is measured in x-ray fluorescence analysis according to claim 1, it is characterized in that, in the time of SUM>SUMS, be less than last time R value again in step 6 R assignment, in the time of SUM<SUMS, be greater than last time R value again in step 6 R assignment.
6. the method for cement composition is measured in x-ray fluorescence analysis according to claim 1 or 5, it is characterized in that, in step 6, again giving the scope of the step-length of R assignment is 0.001-0.1.
7. an X-ray fluorescence analyzing system, comprises data processing equipment, it is characterized in that, described data processing equipment executes claims step 4 in the method described in 1-6 any one to step 6.
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| RU200118U1 (en) * | 2020-07-15 | 2020-10-07 | Дмитрий Алексеевич Гришко | MONITOR BLAST CEMENTATION NOZZLE |
| RU2757545C1 (en) * | 2021-03-16 | 2021-10-18 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Волгоградский государственный технический университет" (ВолгГТУ) | Method for determining the amount of cement in a product made of a cement-sand mixture |
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