CN105241907A - Method for analyzing pig iron components through X-ray fluorescence spectrometry - Google Patents
Method for analyzing pig iron components through X-ray fluorescence spectrometry Download PDFInfo
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- CN105241907A CN105241907A CN201510760656.8A CN201510760656A CN105241907A CN 105241907 A CN105241907 A CN 105241907A CN 201510760656 A CN201510760656 A CN 201510760656A CN 105241907 A CN105241907 A CN 105241907A
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Abstract
The invention relates to a method for analyzing pig iron components through X-ray fluorescence spectrometry. The method includes the steps that a pig iron sample is smashed until pig iron sample powder can pass through 0.125 mm screen cloth, the pig iron sample powder is mixed evenly, and the optimal working conditions of a sample pressing machine, the optimal analysis spectral lines of all elements and the corresponding optimal working parameters of a spectrograph are set; boric acid is adopted as a setoff material for manufacturing a boric acid substrate and a boric acid surrounding edge of pressed powder pellets; each pressed powder pellet is closely wrapped by a preservative film uniform in texture; analysis programs of all the elements are manufactured by adopting a calibration curve method, characteristic X-ray intensity of all the elements is measured to set up a final analysis program and a drift correction program, the sample is analyzed after drift correction and verification analysis are carried out on the spectrograph, and averages are calculated to report results on the condition that deviations between parallel sample detection results do not exceed the allowance range. By means of the method, the various elements such as silicon, manganese, phosphorus, nickel, chromium, copper, arsenic, vanadium, titanium and stannum in pig iron can be analyzed at a time, the analysis results are directly read out from a computer, operation is easy, and the analysis speed is high.
Description
Technical field
This method belongs to X-ray fluorescence spectra analytic approach, is a kind of method that X-ray fluorescence spectra analyzes pig iron composition.
Background technology
Adopt the chemical analysis method of wet method to analyze the chemical composition of the pig iron traditionally, measure the content of wherein different element according to different chemical principles respectively.Along with the development of instrument manufacturing technology and analysis software, the analytical instrument such as atomic absorption spectrophotometer (AAS), Xray fluorescence spectrometer, photo-electric direct reading spectrometer, ICP emission spectrometer are applied more and more wider in the analysis of the pig iron.In these instrument analytical methods, except elimination of Blank for Analysis is only applicable to the block pig iron, other several instrument analytical methods all can be used for the analysis of the powdery pig iron.And wherein wavelength dispersion X-ray fluorescence spectrometry, because sample preparation is relatively simple, do not need to use the hazardous chemical such as acid, alkali, can Simultaneously test Multiple components, precision, the accuracy of method are better, are more and more vast analytical work person acceptance.
Utilize the method for the block pig iron of Xray fluorescence spectrometer Direct Analysis to have CNS GB/T223.79-2007 " the mensuration x-ray fluorescence spectrometry method of the many cellulose contents of iron and steel ", but utilize the method for the Xray fluorescence spectrometer Direct Analysis powdery pig iron to there is no national standard, international standard or industry standard.Some periodicals exchange forum with analytical technology have paper about the Xray fluorescence spectrometer Direct Analysis powdery pig iron, and the method for these papers is nothing more than two classes: after adding additives, pressed powder-X-fluorescence measures or directly pressed powder-X-fluorescence measures.The former makes pressed powder after pig iron powder and bonding reagent being mixed by a certain percentage, put into X fluorescence spectrometer again to detect, this method needs to use bonding reagent as methylcellulose etc., sample and cementing agent all need precise and fully mix, cumbersome like this and waste time, and once mix uneven meeting to have a strong impact on the precision of analysis and the accuracy of result.A kind of rear method is that pig iron direct powder compression is put into X-fluorescence direct-detection again.But especially gray iron cohesiveness is very poor for a lot of pig iron, even if be pressed into disk reluctantly, disk is once enter spectrometer, under the negative pressure of spectrometer strong vacuum, disperse immediately in disk sample face, causes spectrometer vacuum chamber contaminated simultaneously, cause damage to instrument; Some pig iron does not have cohesiveness even at all, at all cannot compression molding, thus just cannot adopt yet and analyze in this way.
Summary of the invention
The present invention aims to provide a kind of method that X-ray fluorescence spectra analyzes pig iron composition, solve the problem utilizing the Xray fluorescence spectrometer Direct Analysis powdery pig iron, overcoming prior art can not direct tablet compressing and need precise and add cementing agent and the shortcoming of fully mixing to the very poor powdery pig iron of cohesiveness, realize powdery pig iron direct tablet compressing and single-time measurement goes out the content of the various compositions such as silicon, manganese, phosphorus, nickel, chromium, copper, arsenic, titanium, vanadium, tin, reduce operational loaded down with trivial details, improve analysis speed, and avoid causing analytical instrument stained.
Object of the present invention is achieved through the following technical solutions:
By the method for x ray fluorescence spectrometry express-analysis pig iron composition, the steps include:
(1) prepare before analyzing: pig iron sample was crushed to 0.125mm screen cloth and mixes, the working pressure 35 ~ 55 tons of pressure-like machine, 25 ~ 45 seconds dwell times are set, select the Ka spectral line of each element or Kb spectral line as analytical line, select the 2 θ angles corresponding with spectral line simultaneously, the light pipe voltage 30 ~ 60KV of X-fluorescence, tube current 40 ~ 80mA;
(2) pressed powder is made: utilize powdered sample pressure-like machine and boric acid powder to produce boric acid substrate and surrounding edge, the pressed powder of the pig iron is exposed in upper surface middle part, sheeting thickness is 4 ~ 8mm, wherein pig iron sample thickness 0.3 ~ 0.6mm, and the diameter of pig iron exposed area is 30 ~ 32mm;
(3) preservative film parcel: pressed powder is closely wrapped up with homogeneous preservative film;
(4) X-fluorescence detects:
With a series of powdery pig iron standard specimen or control sample by the control sample of chemical definite value, by step (1) ~ (3) sample preparation with arrange running parameter, X fluorescence spectrometer measures the characteristic X ray strength of element, through background correction and matrix correction, produce the working curve of the characteristic x-ray fluorescence intensity-content of each element;
The method that the drift correction sample of instrument also adopts preservative film to wrap up and standard specimen or control sample and synchronously detect and arrange, and then set up final routine analyzer and drift correction program;
Before analytical sample, first with drift correction sample, drift correction is carried out to spectrometer;
After drift correction, carry out check analysis, to judge whether drift correction puts in place, the need of further adjustment with standard specimen or control sample;
Drift correction or after adjusting to the right place, sample is put into spectrometer and detects, coupon results is calculated by working curve relational expression;
(5) analysis result is reported: judge whether the deviation between parallel sample testing result exceeds tolerance, as overproof, again detect with the routine analyzer built up in X fluorescence spectrometer by step (1) ~ (3) sample preparation, as not overproof, average and quote analysis result.
The invention has the advantages that, can directly analyze the powdery pig iron and the disposable content analyzing the multiple elements such as silicon, manganese, phosphorus, nickel, chromium, copper, arsenic, titanium, vanadium, tin, and simple, quick to analyzing the whole process operation of result from sample preparation, can not cause stained to analytical instrument.
Accompanying drawing explanation
Accompanying drawing is analytical procedure figure.
Embodiment
The following provide of the present invention one group 10 and analyze embodiment:
1 analyzes front preparation
1.1 samples are pulverized: with comminutor, pig iron sample was crushed to 0.125mm screen cloth, and fully mixes, and load and have filled in the sample bag of specimen coding.
1.2 pressure-like machines prepare: arrange working pressure 40 tons, 30 seconds dwell times.
1.3X fluorescence spectrophotometer prepares: specify to select the analysis condition of each element and corresponding X fluorescence spectrometer running parameter by table 1, and unified selection " sample rotation " function.Other conditions are as analyzed material requested kind and specification, and instrumental working conditions, preheating, spot check and correction etc., perform by the conventional analysis of X fluorescence spectrum spectrometer.
2 make pressed powder
Wipe clean with medical cotton the dust that sample cup inwall contained by pressure-like machine, dip in plane and position-limiting drum inwall on the clean piston of wipes of alcohol with medical cotton.Put position-limiting drum (internal diameter 31mm) well, decline piston is to position-limiting drum screens.With sample spoon, pig iron powder is being contained sample cup basal surface and complete uniform fold along position-limiting drum inner core spreading, spreading thickness is about 0.6mm, then in pig iron powder surface and whole sample cup, the half position of boric acid powder to sample cup volume is put into, remove position-limiting drum, put into boric acid powder again, boric acid powder on pressure-like machine workbench to be swept in Piston mould and floating, final boric acid powder position is to from sample cup about 1mm suitable for reading.Cover gland, tension pressure-like machine rocking arm, make plane and the alignment of upper prop bottom surface on piston, start piston rising switch, now piston rises, and to specifying 40 tons of pressure, pressurize is after constant 30 seconds, and piston declines automatically.Pushing rocking arm open, again starting piston rising switch to ejecting disk.The wafer thickness made is about 6mm, and wherein pig iron sample thickness is about 0.5mm, and the diameter of pig iron exposed area is 31mm.
Each sample production two pressed powders.
3 preservative film parcels
The disk have gentle hands pressed is comforted the boric acid burr removing periphery, then blow away the floating ash on print surface with rubber pipette bulb.Select quality and the uniform preservative film of thickness, the fritter that clip is of moderate size covers disk surfaces, is tightened up by preservative film and paste with self-adhesive label paper fixing at the back side in the face of analysis.Wherein, analyze between the preservative film in face and disk and must contact closely, non-wrinkled, without bubbling, more must not breakage be had, otherwise, must again wrap up.On self-adhesive label paper, sample number into spectrum is finished writing after parcel.
4X fluoroscopic examination
4.1 standard specimens and control sample are selected: choose 9 powdery pig iron standard specimens, adopt chemical analysis to carry out definite value to not having the element of definite value.In addition, the content range of Partial Elements is too narrow, therefore also adopts chemical analysis to carry out definite value from producing sample the sample selecting 6 content suitable.Standard specimen and control sample finally for setting up working curve amount to 15.
4.2 background deductions: adopt a series of block pig iron standard substance, using preservative film and carrying out strength detection and energy scan under not using preservative film to wrap up two kinds of situations respectively, according to the difference of the intensity in two kinds of situations and energy scan, according to the running program of X fluorescence spectrometer button background software, background deduction is carried out to each element, thus the background interference that elimination preservative film brings.
4.3 calibration curves make: according to step 1-3 sample preparation with arrange analytical parameters, sample making two compressing tablets of each numbering, the information such as numbering, constituent content of input standard specimen and control sample, measure the characteristic X ray strength of each element of each sample one by one, and according to step 4.2 background correction, each sample measures 2 times, and the final characteristic X ray strength of the element of each sample is averaged.The mean value of standard specimen and the control constituent content value of sample and the x-ray fluorescence intensity of measurement is drawn calibration curve, then carries out Theoretical Alpha correction, obtain final working curve.
The setting of 4.4 drift correction samples: with two blocks of block pig iron (concentration of element is respectively close to the upper and lower limit of calibration curve) standard specimen, with preservative film parcel, with above-mentioned powder standard substance Simultaneous Determination intensity.This wraps up the drift correction sample of block pig iron standard specimen as this analytical approach of preservative film.
For the preservative film quality difference of elimination different batches is to analyzing the systematic bias impact brought, when making calibration curve, the preservative film of same batch is adopted to carry out parcel and and standard specimen Simultaneous Determination to drift correction sample.
The analysis of 4.5 unknown samples
4.5.1 instrument drift corrects: drift correction sample is put into X fluorescence spectrometer successively, selects drift correction program determination to correct the characteristic X ray strength of each element of sample, and computing machine calculates correction factor according to initial strength when measuring intensity and creation facilities program (CFP).
Often change a collection of preservative film, the preservative film after replacing must be adopted to carry out drift correction and checking mensuration to after drift correction sample, checking standard specimen or control sample parcel to X fluorescence spectrometer.
4.5.2 check analysis: select two standard specimens or control sample (constituent content is respectively more than less than 1/3 of analyst coverage and 2/3) to measure its content according to after step 1-3 sample preparation.After measurement result and scale value or reference value are coincide, then analytical sample; If measurement result exceeds permissible error, then again carry out drift correction and check analysis, until measurement result and scale value or reference value are coincide.Put in place if repeatedly correct still cannot correct, manually can adjust response curve.
4.5.3 sample analysis: by sample according to after step 1-3 sample preparation, put into instrumentation sample dish in order, analysis computer chooses routine analyzer and analysis task, startup analysis program, Direct Analysis goes out the concentration of each element in sample.Analysis result is directly read by computing machine.
5 report analysis results
Sample detects and terminates, and judges whether the testing result between parallel sample exceeds permissible error scope.As not overproof, average and quote analysis result; As overproof, then again detect by step 1 ~ 3 sample preparation.
If again sample preparation and analyze after, whether parallel analysis result is still overproof, then from the homogeneity and sample making course of sample, have pollution to investigate and analyse to sample.
The analyzing crystal of table 1 analytical line, recommendation, 2 θ angles, light pipe electric current and voltage and possible interference element
Claims (1)
1., by the method for x ray fluorescence spectrometry express-analysis pig iron composition, it is characterized in that comprising the following steps:
(1) prepare before analyzing: pig iron sample was crushed to 0.125mm screen cloth and mixes, the working pressure 35 ~ 55 tons of pressure-like machine, 25 ~ 45 seconds dwell times are set, select the Ka spectral line of each element or Kb spectral line as analytical line, select the 2 θ angles corresponding with spectral line simultaneously, the light pipe voltage 30 ~ 60KV of X-fluorescence, tube current 40 ~ 80mA;
(2) pressed powder is made: utilize powdered sample pressure-like machine and boric acid powder to produce boric acid substrate and surrounding edge, the pressed powder of the pig iron is exposed in upper surface middle part, sheeting thickness is 4 ~ 8mm, wherein pig iron sample thickness 0.3 ~ 0.6mm, and the diameter of pig iron exposed area is 30 ~ 32mm;
(3) preservative film parcel: pressed powder is closely wrapped up with homogeneous preservative film;
(4) X-fluorescence detects:
With a series of powdery pig iron standard specimen or control sample by the control sample of chemical definite value, by step (1) ~ (3) sample preparation with arrange running parameter, X fluorescence spectrometer measures the characteristic X ray strength of element, through background correction and matrix correction, produce the working curve of the characteristic x-ray fluorescence intensity-content of each element;
The method that the drift correction sample of instrument also adopts preservative film to wrap up and standard specimen or control sample and synchronously detect and arrange, and then set up final routine analyzer and drift correction program;
Before analytical sample, first with drift correction sample, drift correction is carried out to spectrometer;
After drift correction, carry out check analysis, to judge whether drift correction puts in place, the need of further adjustment with standard specimen or control sample;
Drift correction or after adjusting to the right place, sample is put into spectrometer and detects, coupon results is calculated by working curve relational expression;
(5) analysis result is reported: judge whether the deviation between parallel sample testing result exceeds tolerance, as overproof, again detect with the routine analyzer built up in X fluorescence spectrometer by step (1) ~ (3) sample preparation, as not overproof, average and quote analysis result.
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