CN101526488A - Method for analyzing components of iron ore by using X-ray fluorescence spectrum - Google Patents
Method for analyzing components of iron ore by using X-ray fluorescence spectrum Download PDFInfo
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- CN101526488A CN101526488A CN200810030732A CN200810030732A CN101526488A CN 101526488 A CN101526488 A CN 101526488A CN 200810030732 A CN200810030732 A CN 200810030732A CN 200810030732 A CN200810030732 A CN 200810030732A CN 101526488 A CN101526488 A CN 101526488A
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Abstract
The invention discloses a method for analyzing the components of iron ore by using an X-ray fluorescence spectrum, which comprises before-analysis preparation (1) and analysis report submission (5), and the steps between the before-analysis preparation (1) and the analysis report submission (5) including molten sample manufacturing (2), detection by an internal standard method (3) and analysis by a calibration curve method (4), wherein in the before-analysis preparation (1) step, a working curve (16) is built; in the detection by an internal standard method (3) step, an internal standard line of a molten sample is measured; and in the analysis by a calibration curve method (4) step, the measurement results of the molten sample are obtained. The method completes the measurement of all elements in the iron ore by melting once, is high in measurement accuracy, simplifies process and time for measurement, reduces cost of the analysis of the components of the iron ore, and is suitable to be applied to the iron and steel industry and researches.
Description
Technical field
The present invention relates to a kind of method of iron ore chemical composition analysis, particularly relate to a kind of employing fusion method iron ore is melt into glass sheet, the method for the X-ray fluorescence spectra analyzing components of iron ore of various chemical composition contents such as the full iron in the use Wavelength dispersion type x ray fluorescence spectrophotometer Measurement and analysis iron ore, calcium oxide, magnesium oxide, silicon dioxide, sulphur, phosphorus, titania, alchlor, manganese oxide, vanadium pentoxide.
Background technology
Traditional iron ore chemical analysis method is to adopt different elements are carried out the content that specific chemical reaction is measured its chemical constitution respectively.Along with popularizing gradually of instrumental analysis in recent years, X fluorescence spectrophotometer, ICP emission spectrometer are used more and more extensivelyr in the analysis of iron ore, especially wavelength dispersion X-fluorescence method, because its pre-treatment is simple relatively, can measure multiple composition simultaneously, advantages such as the precision of method, accuracy are better more and more are that vast iron ore analytical work person accepts.
Each class standard that utilizes the X fluorescence spectrophotometer to analyze iron ore is at present successively put into effect, international standard ISO9516:1992 " iron ore---silicon, calcium, manganese, aluminium, titanium, magnesium, phosphorus, sulphur and potassium---wavelength dispersion X-ray fluorescence spectrometry " is arranged, CNS GB/T6730.62-2005 " iron ore---calcium, silicon, magnesium, titanium, phosphorus, manganese, aluminium and barium Determination on content---wavelength dispersion X-ray fluorescence spectrometry ".These two kinds of methods all are to use pure material to carry out proportioning according to the ratio of iron ore heterogeneity, by different bearing calibrations absorption enhancement effect, matrix effect etc. are carried out mathematics again and proofread and correct, and the computed in software by special use goes out analysis result at last.But all there are some shortcomings in these two kinds of methods: the accuracy that can not guarantee to measure ferro element after the fusion, and ferro element is a most important element in the iron ore, basic each iron ore sample all will be analyzed ferro element, this just means the content that also will measure ferro element after using standard method to analyze iron ore with additive method again, and is cumbersome; Adding when taking off grinding agent or oxygenant before the fusing sample all is to add after the accurate respectively weighing of each sample, bothersome time-consuming; After sample analysis is finished, re-use special-purpose computer program after the fluorescence intensity of each element of measuring must being printed and calculate just and can draw final analysis result, can not use accompanying software to calculate, troublesome poeration is easily made mistakes.
In addition, what most of fluorescence users used is that working curve method is analyzed each element in the iron ore, after being about to serial standards for iron ore sample melted and becoming glass sheet, different elements is set up working curve respectively, also used different bearing calibrations to revise absorption enhancement effect, matrix effect etc. simultaneously.Substantially can use the function software of standard of instruments configuration directly to obtain analysis result although it is so, and need not calculate again, have more general applicability, but still can not solve the problem that ferro element accurately analyzes and the problem of weighing repeatedly by other software.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of the realization to finish the measurement of full iron, calcium, magnesium, silicon, sulphur, phosphorus, titanium, aluminium, manganese, content of vanadium after the fusion, thereby solve the method for the X-ray fluorescence spectra analyzing components of iron ore of the analysis of most important ferro element in the iron ore.
Purpose of the present invention is achieved by following technical proposals:
Inventive method of the present invention comprises analyzes the preceding analysis report of preparing and submit to.Preparing before the described analysis and submitting the method step between the analysis report to is that fusing sample is made, internal standard method detects and the calibration curve analysis; Preparatory stage is set up working curve before analysis, records the internal standard line of fusing sample ferro element at the internal standard method detection-phase, obtains the measurement result of fusing sample in the calibration curve analysis phase.
It is that employing X fluorescence spectrophotometer is measured the FeK in the fusing sample respectively add a cobalt element of determining to measure in fusing sample after that described internal standard method detects
β 1,3Value and CoK
α 1,2Value is with CoK
α 1,2Value is as FeK
β 1,3The internal standard line of value.
Described calibration curve analysis is that the fluorescence intensity that adopts the X-ray fluorescence spectra analyser to obtain serial each element of standard specimen is kept in the computing machine and sets up standard specimen intensity---the content working curve, wherein ferro element then is to adopt internal standard method promptly to use serial standard specimen FeK
β 1,3/ CoK
α 1,2Value the content of standard specimen ferro element is done calibration curve, last coupon results is calculated by working curve and is got.
Described fusing sample making comprises sample, dropping oxidizing agent and release agent in the step mixing crucible, waves the mixing fusing sample, pours sample in the mould moulding and cooling fusing sample.
Prepare to comprise the preparation of step reagent, dry sample, instrument and equipment preparation, pulverizing, mixing, calcination flux before the described analysis, dry cobalt oxide, set up working curve, instrument drift is proofreaied and correct, the preparation of cleaning platinum yellow crucible and mould and release agent and oxygenant.
Described reagent prepares to comprise that the mixing P10 gas by the methane of 90% argon gas and 10% that is used for the gas proportional counter prepares; 67: 33 mixed fluxs of pure lithium tetraborate of top grade or lithium tetraborate and lithium metaborate are prepared, and dry by the fire 4 hours down at 500 ℃, place the exsiccator cooling standby; Cobalt sesquioxide, top grade is pure, dries by the fire 1h down at 105 ℃, places the exsiccator cooling standby; LiNO
3=400g/L or NaNO
3=400g/L and LiBr=400g/L or NH
4The I=400g/L mixed solution; Taking by weighing 400.0g analyzes pure lithium nitrate or sodium nitrate and 400.0g and analyzes pure lithium bromide or the iodate ammonia 1000mL of being diluted to soluble in water; HNO
3=1+5 volume ratio.
Compared with prior art, the present invention has the following advantages: the measurement of all elements in the iron ore is finished in a fusion, and the measuring accuracy height, has simplified process of measurement and time, has reduced the cost that components of iron ore is analyzed.The present invention is fit to iron and steel enterprise and research institute uses.
Description of drawings
Fig. 1 is the method flow synoptic diagram of one embodiment of the invention.
Embodiment
The invention will be further described below in conjunction with drawings and Examples:
With reference to Fig. 1, the present invention includes and analyze preceding preparation 1 and submission analysis report 5, the method step before the described analysis between preparation 1 and the submission analysis report 5 is that fusing sample making 2, internal standard method detection 3 and calibration curve analyze 4; 1 stage of preparing before analysis is set up working curve 16, detects the internal standard line that 3 stages recorded fusing sample in internal standard method, analyzes 4 stages acquisition fusing sample measurement result at calibration curve.
It is that employing X fluorescence spectrophotometer is measured the FeK in the fusing sample respectively add a cobalt element of determining to measure in fusing sample after that described internal standard method detects 3
β 1,3Value and CoK
α 1,2Value is with CoK
α 1,2Value is as FeK
β 1,3The internal standard line of value.
Described calibration curve analysis 4 is that the fluorescence intensity that adopts the X-ray fluorescence spectra analyser to obtain serial each element of standard specimen is kept in the computing machine and sets up standard specimen intensity---the content working curve, wherein ferro element then is to adopt internal standard method promptly to use serial standard specimen FeK
β 1,3/ CoK
α 1,2Value the content of standard specimen ferro element is done calibration curve, last coupon results is calculated by working curve and is got.
Described fusing sample make 2 comprise step be mixed sample 21, dropping oxidizing agent and release agent 22 in the crucible, wave mixing fusing sample 23, pour sample in the mould moulding 24 and cooling fusing sample 25.
Prepare 1 to comprise that step reagent prepares 11 before the described analysis, dry sample 12, instrument and equipment prepare 13, pulverizing, mixing, calcination flux 14, oven dry cobalt oxide 15, set up that working curve 16, instrument drift proofread and correct 17, the preparation 19 of cleaning platinum yellow crucible and mould 18 and release agent and oxygenant.
Described reagent is prepared 11 and is comprised that the P10 gas by the methane blended of 90% argon gas and 10% that is used for the gas proportional counter prepares; Pure lithium tetraborate of top grade or lithium tetraborate and lithium metaborate 67+33 mixed flux are prepared, and dry by the fire 4 hours down at 500 ℃, place the exsiccator cooling standby; Cobalt sesquioxide, top grade is pure, dries by the fire 1h down at 105 ℃, places the exsiccator cooling standby; LiNO
3=400g/L or NaNO
3=400g/L and LiBr=400g/L or NH
4The I=400g/L mixed solution; Take by weighing pure 400.0g lithium nitrate of analysis or sodium nitrate and 400.0g and analyze pure lithium bromide or the iodate ammonia 1000mL of being diluted to soluble in water; HNO
3=1+5 volume ratio.
Described calibration curve analysis 4 is carried out in disposing the computing machine of special software, is calculating before the correct result, and computing machine also carries out to judge whether parallel result exceeds error range 41, carries out then and calculates parallel sample average result 42.
Method of the present invention is applicable to the analysis (table 1) of the little iron ore of calcination loss, pellet, sintering deposit, iron scale screen underflow.
The chemical element measurement range of table 1 embodiment
| Element | Measurement range, % (m/m) | Element | Measurement range, % (m/m) |
| TFe | 20.00～72.00 | Al 2O 3 | 0.50～14.00 |
| CaO | 0.50～15.00 | TiO 2 | 0.10～20.00 |
| MgO | 1.00～10.00 | V 2O 5 | 0.025～0.75 |
| SiO 2 | 1.00～35.00 | P | 0.010～0.500 |
| S | 0.050～2.00 | MnO | 0.050～1.00 |
The analytical line that method of the present invention relates to, analyzing crystal, 2 θ angles, light pipe electric current and voltage and the possible parameters (table 2) such as interference element of recommending use.
The correlation parameter of table 2 embodiment
| Element | Spectral line | Crystal | 2 θ angles, degree | The light pipe electric current and voltage | Possible interference element |
| Fe | FeK β1，3 | LiF200 | 51.77 | 30KV～80mA | Co |
| Ca | CaK α1，2 | LiF200 | 113.09 | 30KV～80mA | --- |
| Mg | MgK α1，2 | AX06 | 18.97 | 30KV～80mA | Ca、Br |
| Si | SiK α1，2 | PET | 109.03 | 30KV～80mA | |
| S | SK α1，2 | Ge(111) | 110.69 | 30KV～80mA | |
| P | PK α1，2 | Ge(111) | 141.04 | 30KV～80mA | Cu |
| Al | AlK α1，2 | PET | 144.65 | 30KV～80mA | Cr、Ti、Br |
| Ti | TiK α1，2 | LiF200 | 86.17 | 30KV～80mA | --- |
| V | VK α1，2 | LiF200 | 76.93 | 30KV～80mA | Ti |
| Mn | MnK α1，2 | LiF200 | 62.97 | 30KV～80mA | Cr、Fe |
| Co | CoK α1，2 | LiF200 | 52.79 | 30KV～80mA | Fe |
Embodiment:
Reagent and material: P10 gas, the mixed gas that argon gas by 90% and 10% methane are formed is used for the gas proportional counter.
Flux: pure lithium tetraborate of top grade or lithium tetraborate and lithium metaborate 67+33 mixed flux, dried by the fire 4 hours down at 500 ℃, place the exsiccator cooling standby.
Cobalt sesquioxide, top grade is pure, dries by the fire 1h down at 105 ℃, places the exsiccator cooling standby.
[LiNO
3=400g/L or NaNO
3=400g/L and LiBr=400g/L or NH
4I=400g/L] mixed solution: take by weighing 400.0g and analyze pure lithium nitrate or sodium nitrate and 400.0g and analyze pure lithium bromide or the iodate ammonia 1000mL of being diluted to soluble in water.
HNO
3: the 1+5 volume ratio.
Xray fluorescence spectrometer: formula wavelength dispersion spectrometer simultaneously or sequentially, satisfy the regulation of " JJG810 People's Republic of China (PRC) national metrological verification regulations wavelength dispersion X-ray fluorescence spectrometer ".The X-ray tube of high-purity element target.
Analyzing crystal: all elements in can covering method, can use the crystal of plane or flexure plane.
Collimating apparatus:, should select suitable collimating apparatus for the sequence type instrument.Thick collimating apparatus is used for the analysis of the light element of atom sequence number＜22.Thin collimating apparatus is used for the analysis of the heavy element of atom sequence number 〉=22.
Detector: scintillation counter is used for the analysis of heavy element; The gas proportional counter is used for the analysis of light element; Also can use the sealing proportional counter.
Vacuum system: in the measuring process, vacuum system must be maintained to the following constant compression force of few 30Pa.
Measuring system: the unify special software of configuration of department of computer science can calculate the content of each element according to measured intensity.
The high temperature sample-melting stove: the high temperature sample-melting stove can be kept 1100 ℃ at least, preferably can wave automatically.
Platinum yellow gold crucible or mould: with the supporting use of sample-melting stove, the mould bottom surface is smooth smooth, and it is suitable to water the glass sheet size, the thickness that cast out.
Sampling: press GB/T10322.1-2000 sampling, sample preparation.Should in exsiccator, be cooled to room temperature 105 ℃～110 ℃ oven dry before the sample analysis.
The general preparation process of fuse piece: the sample that will cross 120 mesh sieves and oven dry respectively, claim 0.5000g～0.7000g accurately to 0.0002g, cobalt sesquioxide 0.1000g is accurately to 0.0002g, put into and weigh up 7.0000g accurately to the platinum yellow gold crucible of 0.0005g flux, with glass bar carefully with sample and flux mixing, and the sample that glass bar is attached, flux sweeps crucible, evenly join the mixed solution of 1.00mL in the sample, put into pre-oxidation 1min on the sample-melting stove then, crucible is put into the stove that furnace temperature reaches 1050～1100 ℃, wave fusion and cool off after 15 minutes and make the glass fuse piece, carrying out mark, to put into exsiccator to be measured.
Visual inspection: after making the fusion print, whether visual inspection fusion print exists the not defectives such as material, crystallization or bubble of fusion, and defective fusion print should be given up, and prepares qualified fusion print again.
The storage of fusion print: for fear of the suction of the good print of fusion or polluted, to put into exsiccator rapidly behind the molten good print threading sample bag, can not touch with hand and analyze the surface, can not handle by any way, the surface is not analyzed in water or other solvent washings, grinding or polishing especially.
The cleaning of platinum yellow gold crucible or mould: between twice fusion, need clean platinum yellow gold crucible or mould, boil with hot nitric acid and soaked about 15 minutes, after all remaining fused mass of visual inspection all are removed, earlier clean with distilled water flushing again with tap water, use dry back.
The working environment of instrument: the working environment of instrument should satisfy GB/T 16597 x-ray fluorescence spectrometry method general rules.Condition of work: the X-ray spectrometer should make condition of work obtain optimization before measuring by the requirement of apparatus manufacturer, and before measurement preheating 1h or up to instrument stabilizer at least.
Measuring condition:, select suitable measuring condition according to kind, analytical element, coexistence elements and the content scope thereof of employed instrument type, sample.The gate time of analytical element depends on the content of quantitative element and the analytical precision that will reach, and preferred version is 5～60s.The selection of light pipe voltage, electric current should consider to measure the rated power of spectral line lowest excited voltage and light pipe.The preferred pulse altitude selector.When using a plurality of sample box, sample box face shield should not constitute significantly influence to analysis result, and preferred sample box face shield diameter is 20mm～35mm.Preferred sample rotation during measurement.The preferred analytical line that uses, analyzing crystal, 2 θ angles, light pipe electric current and voltage and the possible interference element recommending to use are listed in the accompanying drawing 3, also can use the fixedly road of respective element.
The drafting of calibration curve: under selected condition of work, after choosing some standard substance sample melted similar to analysis specimen, each sample should be measured 2 times at least, and the mean value of the x-ray fluorescence intensity of the content value of analytical element in the standard substance and measurement is drawn calibration curve.Ferro element then is to adopt the cobalt internal standard method, promptly a certain amount of cobalt element is added in the known standard specimen of iron content the FeK of ferro element in the measurement standard test portion
β 1,3With internal standard element CoK
α 1,2The X ray strength ratio, with the relative iron content drawing of this strength ratio curve.
Instrument drift is proofreaied and correct: because the variation of instrument state can cause departing from of measurement result, for directly utilizing original x-ray fluorescence intensity value, before analytical work, use the drift correction sample instrument is carried out drift correction.Can adopt single point correction or two point calibrations, can determine according to the stability of instrument the interval time of correction.
The present invention observes " GB/T 16597 metallurgic product analysis method x ray fluorescence spectrometry general rules " and standardization files such as " JJG 810 People's Republic of China's national metrological verification regulations wavelength dispersion X-ray fluorescence spectrometers ".
Method principle of the present invention: sample is made borate glass shape fusion print by fusion mould notes, available flux has the mixed flux of lithium tetraborate or lithium tetraborate and lithium metaborate, the elementary x-ray irradiation that X-ray light pipe produces is to bright and clean fuse piece surface the time, the secondary characteristic X-ray that produces is after the crystal beam split, and detector is measured its intensity at place, the corresponding 2 θ angles of the characteristic wavelength of selecting.X-transmitted intensity according to calibration curve and measurement, the computer configuration special software calculates full iron, calcium oxide, magnesium oxide, silicon dioxide, sulphur, phosphorus, titania, alchlor, manganese oxide, vanadium pentoxide content in the sample, the automatic output report of computing machine.
Claims (6)
1. the method for an X-ray fluorescence spectra analyzing components of iron ore, comprise and analyze preceding (1) and the submission analysis report (5) prepared, it is characterized in that: the method step of preparing before the described analysis between (1) and the submission analysis report (5) is that fusing sample is made (2), internal standard method detection (3) and calibration curve analysis (4); (1) stage of preparing before analysis is set up working curve (16), detects the internal standard line that (3) stage records fusing sample in internal standard method, obtains the measurement result of fusing sample in calibration curve analysis (4) stage.
2. the method for a kind of X-ray fluorescence spectra analyzing components of iron ore according to claim 1, it is characterized in that: it is that employing X fluorescence spectrophotometer is measured the FeK in the fusing sample respectively add a cobalt element of determining to measure in fusing sample after that described internal standard method detects (3)
β 1,3Value and CoK
α 1,2Value is with CoK
α 1,2Value is as FeK
β 1,3The internal standard line of value.
3. the method for a kind of X-ray fluorescence spectra analyzing components of iron ore according to claim 1 and 2, it is characterized in that: described calibration curve analysis (4) is that the fluorescence intensity that adopts the X-ray fluorescence spectra analyser to obtain serial each element of standard specimen is kept in the computing machine and sets up standard specimen intensity---the content working curve, wherein ferro element then is to adopt internal standard method promptly to use serial standard specimen FeK
β 1,3/ CoK
α 1,2Value the content of standard specimen ferro element is done calibration curve, the analysis result of last fusion sample calculates by the corresponding relation of working curve.
4. the method for a kind of X-ray fluorescence spectra analyzing components of iron ore according to claim 1 is characterized in that: described fusing sample make (2) comprise step be mixed sample (21), dropping oxidizing agent and release agent (22) in the crucible, wave mixing fusing sample (23), sample poured into moulding in the mould (24) and cooled off fusing sample (25).
5. the method for a kind of X-ray fluorescence spectra analyzing components of iron ore according to claim 1 is characterized in that: prepare (1) before the described analysis and comprise that step reagent prepares the preparation (19) that (11), dry sample (12), instrument and equipment are prepared (13), pulverizing, mixing, calcination flux (14), oven dry cobalt oxide (15), set up working curve (16), (17), cleaning platinum yellow crucible and mould (18) and release agent and oxygenant are proofreaied and correct in instrument drift.
6. the method for a kind of X-ray fluorescence spectra analyzing components of iron ore according to claim 5 is characterized in that: described reagent is prepared (11) and is comprised that the mixing P10 gas by the methane of 90% argon gas and 10% that is used for the gas proportional counter prepares; Pure lithium tetraborate of top grade or lithium tetraborate and lithium metaborate are prepared with 67: 33 mixed fluxs, dry by the fire 4 hours down at 500 ℃, place the exsiccator cooling standby; The pure cobalt sesquioxide of top grade dries by the fire 1h down at 105 ℃, places the exsiccator cooling standby; LiNO
3=400g/L or NaNO
3=400g/L and LiBr=400g/L or NH
4The I=400g/L mixed solution; Taking by weighing 400.0g analyzes pure lithium nitrate or sodium nitrate and 400.0g and analyzes pure lithium bromide or the iodate ammonia 1000mL of being diluted to soluble in water; HNO
3=1+5 volume ratio.
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