CN103969272B - The method and system of cement composition are measured in x-ray fluorescence analysis - Google Patents

The method and system of cement composition are measured in x-ray fluorescence analysis Download PDF

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CN103969272B
CN103969272B CN201310036148.6A CN201310036148A CN103969272B CN 103969272 B CN103969272 B CN 103969272B CN 201310036148 A CN201310036148 A CN 201310036148A CN 103969272 B CN103969272 B CN 103969272B
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measured
cement
sample
ray fluorescence
cement sample
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CN201310036148.6A
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CN103969272A (en
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马振珠
刘玉兵
贾庆海
戴平
赵鹰立
闫冉
韩蔚
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中国建材检验认证集团股份有限公司
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Abstract

The invention relates to x-ray fluorescence analysis and measure the method and system of cement composition. Described method comprises: preparation standard cement sample fuse piece and cement sample fuse piece to be measured, and measure X-fluorescence intensity; It is 5 intensity level that each element-intensities that cement sample to be measured is recorded is converted into thinner ratio, calculates the content of the each chemical composition of cement sample to be measured, calculates the content summation of the each chemical composition of cement sample to be measured; And judge the total SUM of content of the each chemical composition of cement sample to be measured and with standard sample in the difference of content summation SUMS of each chemical composition whether in preset range, repeatedly calculate, in the time that described difference is positioned at preset range, the mass fraction that this time calculates is measurement result. Described X-ray fluorescence analyzing system, the data processing equipment that it comprises is carried out some step in said method. Method and system operating process of the present invention is simple and easy to do, is suitable for practicality.

Description

The method and system of cement composition are measured in x-ray fluorescence analysis
Technical field
The present invention relates to a kind of cement composition determination techniques, particularly relate to a kind of XRF that adopts and divideAnalyse the method and system of measuring 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 thinner ratio, then by measuring seriesThe x-ray fluorescence intensity of calibration sample is made working curve. Then melting according to cement sample and fluxMelt the loss on ignition at temperature, according to the requirement of standard thinner ratio, quantitatively take exactly sample and flux,Sample or the loss of flux and the temperature error of molten sample equipment in the inaccurate and molten sample process of any weighingAll can cause error for measurement result with non-uniform temperature. Therefore, to cement series calibration sample,Molten sample equipment, flux loss on ignition and operating personnel's technical ability all has higher requirements.
Because the defect that exists in above-mentioned existing x-ray fluorescence analysis, the inventor actively in additionResearch and innovation, to founding a kind of method that new x-ray fluorescence analysis measures cement composition to improveAbove-mentioned defect.
Summary of the invention
Main purpose of the present invention is, provides a kind of new x-ray fluorescence analysis to measure cement compositionMethod and system, make its operating process more simple and easy to do, thereby be suitable for practicality.
For achieving the above object, the present invention proposes a kind of side of x-ray fluorescence analysis mensuration cement compositionMethod, it comprises:
Step 1, preparation standard cement sample fuse piece, the thinner ratio of this fuse piece is 5;
Step 2, prepares cement sample fuse piece to be measured;
Step 3, measures above-mentioned standard cement sample fuse piece and cement sample to be measured with x-ray fluorescence analyzerThe intensity of each chemical composition corresponding element in fuse piece;
Step 4, each element-intensities cement sample to be measured being recorded according to formula (1) is converted into thinner ratioBe 5 intensity level,
I i , 5 = I i ( ( α i , f + 1 ) ( 1 + R ) - α i , f 5 α i , f + 6 ) - - - ( 1 ) ;
In formula: Ii,5For chemical analysis i corresponding element in the thinner ratio cement sample fuse piece to be tested that is 5X-ray fluorescence intensity, R is the thinner ratio of cement sample fuse piece to be tested, IiFor cement sample to be testedThe x-ray fluorescence intensity of chemical analysis i corresponding element in fuse piece, αi,fFor influence coefficient,
Calculate the content of the each chemical composition of cement sample to be measured according to formula (2),
C i = I i , 5 C i , s I i , s - - - ( 2 ) ,
In formula: CiFor the mass fraction of chemical analysis i in cement sample to be tested, Ii,sFor standard sampleStudy a part x-ray fluorescence intensity for i corresponding element, Ci,sFor the quality of chemical analysis i in standard sample is dividedNumber;
Calculate the content summation SUM of the each chemical composition of cement sample to be measured according to formula (3),
SUM=ΣCi(3);
Step 5, gives R assignment, and calculates chemical analysis in cement sample to be tested according to step 4The mass fraction C of iiAnd the content summation SUM of the each chemical composition of cement sample to be measured, and judgement is treatedThe content of each chemical composition in the content summation SUM of the each chemical composition of survey cement sample and standard sampleWhether the difference SUM-SUMS of summation SUMS is in preset range;
If so, the mass fraction C of chemical analysis i in the above-mentioned cement sample to be tested calculatingiBe measurement result;
If not, perform step 6;
Step 6, repeating step 5, wherein gives R assignment, again when the each chemical composition of cement sample to be measuredContent summation SUM and standard sample in the difference of content summation SUMS of each chemical composition at default modelEnclose when interior the mass fraction C that this time calculatesiBe measurement result.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, in described step 2The thinner 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, in described step 5,Giving R assignment is for the first time 5.
Preferably, the method for cement composition, described preset range are measured in aforesaid x-ray fluorescence analysisFor-0.05%-0.05%.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, works as SUM > SUMSTime, be less than last time R value again in step 6 R assignment, in the time of SUM < SUMS, in step 6Be greater than last time R value again to R assignment.
Preferably, the method for cement composition is measured in aforesaid x-ray fluorescence analysis, in step 6, again givesThe 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 numberAccording to treating apparatus, described data processing equipment is carried out aforesaid x-ray fluorescence analysis and is measured cement compositionMethod in step 4 to step 6.
By technique scheme, cement is measured in the x-ray fluorescence analysis that the embodiment of the present invention providesThe method and system of composition, in the time preparing sample to be tested fuse piece, without sample and flux are weighed,Melt temperature and time is also without strict demand, only need get a strockle flux and little scoop sample product are put into moltenAfter mixing in the crucible that sample is used, under the arbitrary temp between 950 DEG C~1200 DEG C, melt to range estimationMelt clarification can be made into bead; Also special without employing XRF analysis while making working curveSeries standard sample, with can the finish the work making of curve of a common cement standard sample. FromAnd reduced Operating Complexity and the high request to performance accuracy, make test job simple.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, of the present invention in order to better understandTechnological means, and can be implemented according to the content of description, detailed with preferred embodiment of the present inventionIllustrate as after.
Brief description of the drawings
Fig. 1 is the meter that the present invention proposes method one embodiment of x-ray fluorescence analysis mensuration cement compositionCalculate process flow diagram flow chart.
Detailed description of the invention
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, the x-ray fluorescence analysis proposing according to the present invention is measured to cement compositionIts detailed description of the invention of method and system be described in detail as follows.
The preparation method of fuse piece
1, standard sample fuse piece preparation
The standard cement sample fuse piece that preparation thinner ratio is 5, has accurately taken card cement standard sample msGram (calcination base), and 5ms gram of flux (calcination base) puts into Pt95-Au5 crucible, uses glass barSample in crucible and flux are carefully uniformly mixed. Melting 5 in high temperature furnace more than 950 DEG CMinute above melt completely to sample, pour into and be preheating in 900 DEG C of above Pt95-Au5 molds,Be chilled to after room temperature, take off in drier and preserve.
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 sample, available other estimatorTool is estimated as counter balance) and a strockle flux (do not differ from 1 gram with the amount of taking of standard sample, availableOther is estimated utensil and estimates as counter balance), melting slab, without the strict temperature of controlling fuse piece withTime, 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
With in two fuse pieces of x-ray fluorescence analyzer measurement standard sample and cement sample to be measured all chemistry becomeThe intensity of part corresponding element, as the intensity of calcium oxide measurement calcium constituent, silica measurement element siliconIntensity, needs silicon, iron, aluminium, calcium, magnesium, potassium, sodium, sulphur, titanium, phosphorus in general cement sampleMeasure with the x-ray fluorescence intensity of 11 elements of manganese, minimum will to silicon, iron, aluminium, calcium, magnesium,Seven elements of potassium and sulphur are measured.
3, the calculating of cement sample chemical analysis to be measured
Determine a series of thinner ratio R of sample fuse piece with method of trials and errors, so back-pushed-type (1) or other is effectiveIt is 5 intensity level I that each element-intensities of sample is converted into thinner ratio by formulai,5
Calculate the content of each chemical analysis in sample by formula (2), calculate in sample and respectively change by formula (3)Study a part sum SUM. When each chemical analysis sum in each chemical analysis sum and standard sample in sampleSUMS equates or in preset range time, the result of corresponding each chemical analysis is correspondenceization in sampleStudy the measurement result of part.
I i , 5 = I i ( ( &alpha; i , f + 1 ) ( 1 + R ) - &alpha; i , f 5 &alpha; i , f + 6 ) - - - ( 1 )
C i = I i , 5 C i , s I i , s - - - ( 2 )
SUM=ΣCi(3)
In formula: Ii,5For the X of i chemical analysis corresponding element in the thinner ratio cement sample fuse piece to be measured that is 5 penetratesLine fluorescence intensity;
R is the thinner ratio of cement sample fuse piece to be measured;
IiFor the x-ray fluorescence intensity of i chemical analysis corresponding element in cement sample fuse piece to be measured;
CiFor the mass fraction of chemical analysis i in cement sample to be measured;
Ii,sFor the x-ray fluorescence intensity of the thinner ratio accurate sample i of the standard chemical analysis corresponding element that is 5;
Ci,sFor the mass fraction of chemical analysis i in the accurate sample of standard;
αi,fFor influence coefficient, can adopt method of the prior art to obtain, also can adopt application number to beThe method of introducing in 2012105744112 patent documentations is measured. For ensureing the abundant of present techniques schemeOpen, 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 the silicate of PI typeCement is tested sample, selects lithium tetraborate as flux, 15 different thinner ratio R's ' of preparationBead. Adopt RIGAKUZSXPrimusIIX ray fluorescence analysis instrument (end window Rh target XRay tube) each bead is carried out to x-ray fluorescence intensity mensuration, obtain respectively becoming in each sampleThe X ray intensity I of dividing '. If each constituent concentration C 'iBe 100, and I ' and R ' * I ' are carried outCrossing initial point does linear regression analysis and obtains K2And K1, can try to achieve the corresponding slope of R ' * I ' is K2With I coupleAnswer slope K1, according to formula αi,f=K2/K1Obtain the flux influence coefficient α of each elementi,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, and its chemical group prejudice table 1 is got the bidSample concentration. Operating process is as follows:
1, French cement more than 60 minutes, is taken out cold in drier 950 degrees Celsius of lower calcinationsBut to room temperature, then accurately take 1.2000 grams and put into Pt95-Au5 with 6.0000 grams of sodium tetraborate fluxIn crucible, mix, in the high temperature furnace of 950 DEG C, melting 15 minutes, pours into and is preheating to more than 900 DEG CPt95-Au5 mold in, be chilled to after room temperature, take off bead and preserve in drier.
2, get approximately 1.2 grams of cement sample to be measured and 6 grams of flux, in high temperature furnace, melt to melt evenAfter clarification, pour into and be preheating in 900 DEG C of above Pt95-Au5 molds, be chilled to after room temperature, take offBead is preserved in drier.
3, the ray fluorescence intensity of each chemical analysis in difference Measurement and calibration sample and cement sample to be measured, knotFruit is in standard specimen intensity in table 1 and sample intensity. Be in 2012105744112 patent documentations by application numberThe thinner ratio correction coefficient measurement result providing is also listed in table 1.
4, according to flow process shown in Fig. 1. Make R=5, with formula (1), formula (2) and formula (3) are counted respectivelyCalculate Ii,5,CiAnd SUM (i=silicon, iron, aluminium, calcium, magnesium, potassium, sulphur and titanium or its oxide), knotFruit is in the row at 1 place of sequence number in table 2. Because SUM value is 106.45, be greater than the summation of standard sample99.20, therefore make R value reduce 0.1, i.e. R=4.9, repeats Ii,5, Ci and SUM calculate, resultIn the row at 2 places of sequence number in table 2. So repay while trying to be calculated to R=4.5, SUM value is 98.90, littleIn the summation 99.20 of standard sample. And then R value is added to 0.01, even R=4.51 repeatsIi,5,CiCalculate with SUM, so repay examination and be calculated to the summation that SUM value is more than or equal to standard sample99.20. If SUM=SUMS, or SUM-SUMS≤0.05%, corresponding this sequence number R value is corresponding denseDegree is the measurement result of each chemical analysis in sample. If SUM-SUMS > 0.05%, this corresponding orderThe mensuration knot that number R value and upper sequence number R value secondary corresponding concentration mean value are each chemical analysis in sampleReally. In this example, cement sample to be measured used is the country-level standard substance GSB03201a of cement, measuresResult and standard results and evaluated error are in table 3. Table 4 is to be 2012105744112 special according to application numberProfit document is to influence coefficient measurement result computational chart.
Table 1: master data table
Composition Al2O3 CaO Fe2O3 MgO K2O SiO2 SO3 TiO2 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
αi,f -0.065 -0.582 -0.866 0.156 -0.403 -0.142 -0.332 -0.870
Table 2 calculated data table
Sequence number R IAl2O3 ICaO IFe2O3 IMgO IK2O ISiO2 ISO3 ITiO2
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 CAl2O3 CCaO CFe2O3 CMgO CK2O CSiO2 CSO3 CTiO2
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 CAl2O3 CCaO CFe2O3 CMgO CK2O CSiO2 CSO3 CTiO2
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 numberi,fCalculatingTable
In table: y=1/ (1+R '); K=(XTX)-1(XTY)
And have: K = K 1 K 2 ; X = I 1 ( 1 - y 1 ) I 1 ... ... I 9 ( 1 - y 9 ) I 9 Y = 100 ( 1 - y 1 ) ..... 100 ( 1 - y 9 )
One embodiment of the present of invention also propose a kind of X-ray fluorescence analyzing system, and it is for to cementSample carries out analytical test, and this X-ray fluorescence analyzing system comprises XRF of the prior artStrength detection device and data processing equipment. In the present embodiment, described data processing equipment is carried outStep 4 in the method for above-mentioned x-ray fluorescence analysis mensuration cement composition is 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, be only preferred embodiment of the present invention, not the present invention made to any formOn restriction, although the present invention disclose as above with preferred embodiment, but not in order to limit thisBright, any those skilled in the art, are not departing within the scope of technical solution of the present invention, when utilizingThe technology contents of above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, is in every caseDo not depart from the content of technical solution of the present invention, according to technical spirit of the present invention, above embodiment is doneAny simple modification, 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 thinner ratio of this fuse piece is 5;
Step 2, prepares cement sample fuse piece to be measured;
Step 3, measures above-mentioned standard cement sample fuse piece and cement sample to be measured with x-ray fluorescence analyzerThe intensity of each chemical composition corresponding element in fuse piece;
Step 4, each element-intensities cement sample to be measured being recorded according to formula (1) is converted into thinner ratioBe 5 intensity level,
I i , 5 = I i ( ( &alpha; i , f + 1 ) ( 1 + R ) - &alpha; i , f 5 &alpha; i , f + 6 ) - - - ( 1 ) ;
In formula: Ii,5For chemical analysis i corresponding element in the thinner ratio cement sample fuse piece to be tested that is 5X-ray fluorescence intensity, R is the thinner ratio of cement sample fuse piece to be tested, IiFor cement sample to be testedThe x-ray fluorescence intensity of chemical analysis i corresponding element in fuse piece, αi,fFor influence coefficient,
Calculate the content of the each chemical composition of cement sample to be measured according to formula (2),
C i = I i , 5 C i , s I i , s - - - ( 2 ) ,
In formula: CiFor the mass fraction of chemical analysis i in cement sample to be tested, Ii,sFor standard sampleStudy a part x-ray fluorescence intensity for i corresponding element, Ci,sFor the quality of chemical analysis i in standard sample is dividedNumber;
Calculate the content summation SUM of the each chemical composition of cement sample to be measured according to formula (3),
SUM=ΣCi(3);
Step 5, gives R assignment, and calculates chemical analysis in cement sample to be tested according to step 4The mass fraction C of iiAnd the content summation SUM of the each chemical composition of cement sample to be measured, and judgement is treatedThe content of each chemical composition in the content summation SUM of the each chemical composition of survey cement sample and standard sampleWhether the difference SUM-SUMS of summation SUMS is in preset range;
If so, the mass fraction C of chemical analysis i in the above-mentioned cement sample to be tested calculatingiBe measurement result;
If not, perform step 6;
Step 6, repeating step 5, wherein gives R assignment, again when the each chemical composition of cement sample to be measuredContent summation SUM and standard sample in the difference of content summation SUMS of each chemical composition at default modelEnclose when interior the mass fraction C that this time calculatesiBe measurement result.
2. the method for cement composition, its spy are measured in x-ray fluorescence analysis according to claim 1Levy and be, in described step 2, the thinner ratio of the cement sample fuse piece to be measured of preparation is 2.5-10.
3. the method for cement composition, its spy are measured in x-ray fluorescence analysis according to claim 1Levy and be, in described step 5, giving R assignment is for the first time 5.
4. the method for cement composition, its spy are measured in x-ray fluorescence analysis according to claim 1Levy and be, described preset range is-0.05%-0.05%.
5. the method for cement composition, its spy are measured in x-ray fluorescence analysis according to claim 1Levy and be, as SUM when SUMS, be less than last time R value again in step 6 R assignment, whenWhen 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 inData processing equipment executes claims step 4 in the method described in 1-6 any one to step 6.
CN201310036148.6A 2013-01-30 2013-01-30 The method and system of cement composition are measured in x-ray fluorescence analysis CN103969272B (en)

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CN105486708A (en) * 2015-12-01 2016-04-13 中国建材检验认证集团股份有限公司 Method for XRF analysis of chemical components of sample, and making method of working curve thereof
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RU2633750C1 (en) * 2017-05-10 2017-10-17 Дмитрий Алексеевич Гришко Method for determination of cement quantity in soil-cement material of structure, made by jet grouting
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