CN103674984A - Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material - Google Patents
Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material Download PDFInfo
- Publication number
- CN103674984A CN103674984A CN201310703019.8A CN201310703019A CN103674984A CN 103674984 A CN103674984 A CN 103674984A CN 201310703019 A CN201310703019 A CN 201310703019A CN 103674984 A CN103674984 A CN 103674984A
- Authority
- CN
- China
- Prior art keywords
- aluminium oxide
- spectral line
- xrf
- standard
- compressing tablet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides a method for measuring the content of aluminum oxide and silicon dioxide in an aluminum-silicon fireproof material. Particularly the method comprises the following steps: preparing two or more standard samples, adopting boric acid as a bonder, and pressing the standard samples into pressed standard sample sheets by a pressure machine; measuring the X-ray fluorescence characteristic spectral line intensity of the pressed standard sample sheets by an X-ray fluorescence spectrophotometer respectively to obtain a standard working curve of the corresponding X-ray fluorescence characteristic spectral line intensity of aluminum oxide and silicon dioxide; using boric acid as the bonder for preparing test materials to be tested into pressed sheets of samples to be tested; measuring the X-ray fluorescence characteristic spectral line intensity of the pressed sheets of the samples to be tested by the X-ray fluorescence spectrophotometer, and reading out the content of aluminum oxide and silicon dioxide in the samples to be tested through the standard working curve. According to the method, the measurement operation is accurate and reliable, the detection range is comprehensive, the use of toxic harmful chemical drugs and the discharge of waste acid liquid are reduced, the detection time is shortened, the manpower consumption is reduced, the operating recommendations are safe and feasible, and the popularization and application are facilitated.
Description
Technical field
The present invention relates to content detection technology, specifically aluminium oxide Al in a kind of mensuration Al-Si Refractory Materials
2o
3with silicon dioxide SiO
2the method of content.
Background technology
For Al in Al-Si Refractory Materials
2o
3, SiO
2the mensuration of content, the detection method of domestic current maturation has two, GB/T6900-2006 Al-Si Refractory Materials chemical analysis method and GB/T3044-2007 white fused alumina, pink fused alumina chemical composition analysis method.The detection method principle of two kinds of standards is basic identical, for Al
2o
3and SiO
2apply respectively different detection methods.First: for Al
2o
3>=97% the conventional residual elements summation of measuring of sample, utilizes poor subtracting to try to achieve, and the method requires must possess each residual content of complete detection (as Fe
2o
3, TiO
2, K
2o, Na
2o, CaO, SiO
2deng) ability, have relatively high expectations.For Al
2o
3the sample of < 97% is used alkaline mixed flux, and 800 ℃ of high-temperature fusion are cleared up, EDTA standard solution titrimetry, and pre-treatment is carried out in hot environment, and operation easier is large, consuming time longer.Second: for SiO
2the sample of < 15%, alkaline mixed flux, 800 ℃ of high-temperature fusion are cleared up, and Photometric Determination, for SiO
2>=15% sample, condenses main amount with cohesion gravimetric determination, and solution residual content molybdenum blue spectrophotometry, obtains SiO after merging
2total content.High-temperature fusion and cohesion weight all have operating process complexity, feature consuming time.Sum up existing ripe detection technique, its accuracy and precision are better, but each project needs to detect separately, and operating process is complicated, round of visits that need to be longer, and the use of simultaneously a large amount of medicines has also increased the discharge of pollutant, unfavorable to environmental protection.My company, through experimental exploring repeatedly, utilizes boric acid for cementing agent, compressing tablet sample preparation, and Xray fluorescence spectrometer is measured Al
2o
3, SiO
2content, pre-treatment operation is relatively simple, testing result is accurately quick, has better application value.
The feature that X-ray fluorescence spectra analytical approach (XRF) has accurately, quick, analyst coverage is wide, be widely used in a plurality of fields such as geology, metallurgy, machine-building, environmental protection and bio-pharmaceuticals, the method is with respect to chemical analysis method, sample pre-treatments is simple, and chemical reagent consumption is few, and discharged waste is few, utilize boric acid and national standard sample to mix, compacting series standard sample, axially viewedplasma is wide, and accuracy and precision are high.But the complete detection method of domestic this method is applied to Al in Al-Si Refractory Materials at present
2o
3, SiO
2assay.
Summary of the invention
The object of the invention is to: propose aluminium oxide Al in a kind of sample preparation is simple, analytical cycle is short, detection accuracy is high Al-Si Refractory Materials
2o
3with silicon dioxide SiO
2content assaying method.
The technical solution adopted in the present invention is:
A method of measuring aluminium oxide and dioxide-containing silica in Al-Si Refractory Materials, comprises the following steps:
-Criterion working curve:
1) prepare 4 above standard models, in described standard model, the shared weight ratio of aluminium oxide and silicon dioxide is different;
2) adopting boric acid is that cementing agent, working pressure machine carry out respectively pressed powder by standard model, makes standard model compressing tablet; The design parameter of pressed powder is as follows: boric acid and treat that the weight mixing ratio of compressing tablet sample is 1:1, and the compressing tablet pressure of pressing machine rises under 30 MPa the compressing tablet pressure at 30 MPa and keeps 50s at 10s;
3) use Xray fluorescence spectrometer, measure respectively the XRF characteristic spectral line intensity of above-mentioned standard model compressing tablet, the design parameter of XRF is as follows: while measuring element aluminum, adopt spectral line K α, crystal PE002,144.745 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; While measuring elemental silicon, adopt spectral line K α, crystal PE002,108.972 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; Then, XRF characteristic spectral line intensity and corresponding aluminium oxide and dioxide-containing silica are carried out to linear regression, obtain respectively the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity;
Aluminium oxide and the dioxide-containing silica of-mensuration sample to be tested:
4), by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator stand-by;
5) use boric acid for cementing agent, test portion to be measured that step 4) is obtained are according to step 2) design parameter carry out pressed powder, make sample to be tested compressing tablet;
6) by the XRF setting parameter in step 3), use Xray fluorescence spectrometer to measure the XRF characteristic spectral line intensity of above-mentioned sample to be tested compressing tablet, and by the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity, read the content of aluminium oxide and silicon dioxide in testing sample.
Described step 2) and 5) in boric acid be the pure boric acid of top grade, before use, after grinding, after sieving, drying, to put into exsiccator standby for 200 orders.
Described step 3) and 6) in the detector gas of Xray fluorescence spectrometer be P-10 gas, the argon gas by 90% and 10% methane blended gas form.
Use 4 kinds of above national certified reference materials, carry out described step 2)～3) sample preparation and detect and analyze, continuous 9 tests, average, optimize the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity.
The beneficial effect that the present invention produces is:
(1) this aspect sensing range Al
2o
3: 0～100%,, SiO
2: 0～50%, cover the Al in Al-Si Refractory Materials comprehensively
2o
3, SiO
2content range.Without the sample for different content scope, select distinct methods.
(2) the present invention greatly reduces the use of poisonous and harmful chemicals and the discharge of spent acid solution.Use standard GB/T/T6900-2006 or GB/T3044-2007 to detect, various chemical reagent are more than 10 kinds, and various spent acid solutions discharges are no less than 5 liters/, and this invention is a small amount of acid reagent that top grade is pure (10g/ item) of using only, there is no discharging of waste liquid.
(3) reduce detection time and manpower consumption, by conventional chemical analysis, with 2 days, foreshortened to approximately 1～2 hour.
(4) use of bonding agent and proportioning advantage: the bonding agent of traditional use has boric acid, cellulose and starch etc., for preventing from reducing the detection limit of method, so bonding agent is all controlled in 20%, but can sacrifice the compactness of compressing tablet itself, cause the surface scattering loss of the energy of X ray, even there is the serious situations such as the surperficial incompleteness of print and dry linting directly impact or interference measurement, occur the obvious reduction of characteristic peak intensity or cannot search peak.Its Al of Al-Si Refractory Materials that this method is measured
2o
3and SiO
2content is higher, and cementing agent and sample ratio are adjusted to 1:1, does not also have the problem that method detection limit is inadequate.Smooth, densification and particle is tiny can guarantee preferably sample preparation quality, overcomes above-mentioned shortcoming.
(5) fluorescent yield of x-ray power setting parameter: Al and Si is low, a little less than luminous power, a little less than detected characteristics peak-to-peak signal, after particularly we heighten binder content ratio, the setting effect of conventional 30KV/90mA is bad, in instrument enabled condition, emissive power is adjusted into 25KV/120mA.Two kinds have all obtained higher detected characteristics peak intensity signal compared with light element, the Detection capability of raising method and detection precision.
Accompanying drawing explanation
Fig. 1 is the standard working curve of the corresponding XRF characteristic spectral line of alumina content intensity;
Fig. 2 is the standard working curve of the corresponding XRF characteristic spectral line of dioxide-containing silica intensity.
Embodiment
The present invention is a kind of method of measuring aluminium oxide and dioxide-containing silica in Al-Si Refractory Materials, comprises the following steps:
1) prepare 4 above standard models, in described standard model, the shared weight ratio of aluminium oxide and silicon dioxide is different;
2) adopting boric acid is that cementing agent, working pressure machine carry out respectively pressed powder by standard model, makes standard model compressing tablet; The design parameter of pressed powder is as follows: boric acid and the mixed weight for the treatment of compressing tablet sample be than being 1:1, and the compressing tablet pressure of pressing machine rises to and under 30 MPa the compressing tablet pressure at 30 MPa, keeps 50s at 10s;
3) use Xray fluorescence spectrometer, measure respectively the XRF characteristic spectral line intensity of above-mentioned standard model compressing tablet, the design parameter of XRF is as follows: while measuring element aluminum, adopt spectral line K α, crystal PE002,144.745 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; While measuring elemental silicon, adopt spectral line K α, crystal PE002,108.972 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; Then, XRF characteristic spectral line intensity and corresponding aluminium oxide and dioxide-containing silica are carried out to linear regression, obtain respectively the standard working curve (as shown in Figure 1, 2) of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity;
4), by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator stand-by;
5) use boric acid for cementing agent, test portion to be measured that step 4) is obtained are according to step 2) design parameter carry out pressed powder, make sample to be tested compressing tablet;
6) by the XRF setting parameter in step 3), use Xray fluorescence spectrometer to measure the XRF characteristic spectral line intensity of above-mentioned sample to be tested compressing tablet, and by the standard working curve of XRF characteristic spectral line intensity and aluminium oxide, dioxide-containing silica, read the content of aluminium oxide and silicon dioxide in testing sample.
Described step 2) and 5) in boric acid be the pure boric acid of top grade, before use, after milling, after sieving, drying, to put into exsiccator standby for 200 orders.
Described step 3) and 6) in the detector gas of Xray fluorescence spectrometer be P-10 gas, the argon gas by 90% and 10% methane blended gas form.
Use 4 kinds of above national certified reference materials, carry out described step 2)～3) sample preparation and detect and analyze, continuous 9 tests are averaged, and optimize the standard working curve of aluminium oxide and silicon dioxide correspondence XRF characteristic spectral line intensity.
In this embodiment, the XRF instrument parameter when sheeter parameter of using during pressed powder of the present invention and mensuration XRF characteristic spectral line intensity is as follows:
Sheeter parameter
| Mixing ratio (boric acid+test portion) | Pressure (MPa) | Rise time (s) | Retention time (s) |
| (1:1) | 30 | 10 | 50 |
In this embodiment, boric acid is the pure boric acid of top grade, before use, puts into exsiccator standby after rear 200 orders of grinding sieve, dry.
XRF instrument parameter
| Element | Spectral line | Crystal | Peak position/° | Detector | Tube current (mA) | Tube voltage (KV) |
| Al | Kα | PE002 | 144.745 | Flow | 160 | 25 |
| Si | Kα | PE002 | 108.972 | Flow | 160 | 25 |
In this embodiment, adopted 6 standard models, be respectively: GBW03115, GSBD52001-92, GSBD44001-92, BY(A) 4-2#, 418# and 413#; Concrete:
A1: aluminium oxide standard model GBW03115, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 28.57%, silicon dioxide SiO
2shared weight ratio is 55.90%;
A2: aluminium oxide standard model GSBD52001-92, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 79.26%, silicon dioxide SiO
2shared weight ratio is 1.49%;
A3: aluminium oxide standard model GSBD44001-92, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 90.58%, silicon dioxide SiO
2shared weight ratio is 4.20%;
A4: aluminium oxide standard model BY(A) 4-2#, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 98.86%, silicon dioxide SiO
2shared weight ratio is 0.012%;
A5: aluminium oxide standard model 418#, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 87.16%, silicon dioxide SiO
2shared weight ratio is 6.19%;
A6: aluminium oxide standard model 413#, national standard material, wherein aluminium oxide Al
2o
3shared weight ratio is 37.12%, silicon dioxide SiO
2shared weight ratio is 44.02%.
In this embodiment, analyze experimental procedure as follows:
1, Criterion working curve:
(1.1) preparation of standard sample: pressing tablet machine setting parameter, A1, A2, A3, A4, A5 and A6 standard model are mixed, carried out after pressed powder according to sheeter parameter and boric acid, correspondence obtains Al#, A2#, A3#, A4#, A5# and A6# standard model compressing tablet, to be measured.
(1.2) press XRF instrument parameter and set, set up routine analyzer (called after Al
2o
3routine analyzer), the XRF characteristic spectral line intensity of above-mentioned six the standard model compressing tablets of sequentially determining Al#, A2#, A3#, A4#, A5# and A6#, and and corresponding aluminium oxide Al
2o
3with silicon dioxide SiO
2content carry out linear regression.Obtain respectively aluminium oxide Al
2o
3standard working curve (as shown in Figure 1) and the silicon dioxide SiO of the corresponding XRF characteristic spectral line of content intensity
2the standard working curve (as shown in Figure 2) of the corresponding XRF characteristic spectral line of content intensity.
2, measure the aluminium oxide Al of sample to be tested
2o
3with silicon dioxide SiO
2content:
(2.1) take test portion: accurately take sample 5.00g, be accurate to 0.01g.
(2.2) mix test portion: the sample of step (2.1) is transferred in mortar, takes 5.00g boric acid and mix, grind and fully mix, treat compressing tablet.
(2.3), compressing tablet: open sheeter, the mixing test portion mixing is proceeded in compression mold, cover compressing tablet lid, pressing tablet machine setting parameter, starts compressing tablet.After compressing tablet completes, open mould, take out the sheet sample suppressing.To be checked.
(2.4), measure testing sample: press XRF instrument parameter and set, enter Al
2o
3routine analyzer, records the XRF characteristic spectral line intensity of sheet sample, the aluminium oxide Al of using (1.2) to set up
2o
3standard working curve (as shown in Figure 1) and the silicon dioxide SiO of the corresponding XRF characteristic spectral line of content intensity
2the standard working curve (as shown in Figure 2) of the corresponding XRF characteristic spectral line of content intensity, obtains aluminium oxide Al in testing sample
2o
3with silicon dioxide SiO
2content.
3, method accuracy validation:
Use existing 6 kinds of national certified reference materials, carry out sample preparation and detect and analyze, continuous 9 tests are averaged.
Accurately and reliably, degree of accuracy, higher than national standard and requirement of experiment, is beneficial to and promotes and use the inventive method as can be seen from the above table.Meanwhile, also can further optimize by the method standard working curve (as shown in Figure 1) and the silicon dioxide SiO of the corresponding XRF characteristic spectral line of aluminium oxide Al 2O3 content intensity
2the standard working curve (as shown in Figure 2) of the corresponding XRF characteristic spectral line of content intensity
Embodiment mono-
Measure Al in Al-Si Refractory Materials
2o
3, SiO
2the method of content, is characterised in that: with boric acid, be cementing agent, and pressed powder, Xray fluorescence spectrometer is measured.
Sheeter parameter
| Mixing ratio (boric acid+test portion) | Pressure (MPa) | Rise time (s) | Retention time (s) |
| (1:1) | 30 | 10 | 50 |
XRF instrument parameter
| Element | Spectral line | Crystal | Peak position/° | Detector | Tube current (mA) | Tube voltage (KV) |
| Al | Kα | PE002 | 144.745 | Flow | 160 | 25 |
| Si | Kα | PE002 | 108.972 | Flow | 160 | 25 |
(1) reagent, using in measuring process is as follows
(1.1), boric acid, top grade is pure, (after milling, 200 orders sieve, and put into exsiccator standby after oven dry)
(1.2), detector gas (P-10), 90% argon gas+10% methane
(1.3), aluminium oxide standard model GBW03115, national standard material (Al
2o
3=28.57%, SiO
2=55.90%)
(1.4), aluminium oxide standard model GSBD52001-92, national standard material (Al
2o
3=79.26%, SiO
2=1.49%)
(1.5), aluminium oxide standard model GSBD44001-92, national standard material (Al
2o
3=90.58%, SiO
2=4.20%)
(1.6), aluminium oxide standard model BY(A) 4-2#, national standard material (Al
2o
3=98.86%, SiO
2=0.012%)
(1.7), aluminium oxide standard model 418#, national standard material (Al
2o
3=87.16%, SiO
2=6.19%)
(1.8), aluminium oxide standard model 413#, national standard material (Al
2o
3=37.12%, SiO
2=44.02%)
(2), sampling: by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator.
(3), analysis experimental procedure is as follows:
(3.1), take test portion: accurately take sample 5.00g, be accurate to 0.01g.
(3.2), mix test portion: the sample of step (3.1) is transferred in mortar, takes 5.00g boric acid (1.1) and mix, grind and fully mix, treat compressing tablet.
(3.3), compressing tablet: open sheeter, the mixing test portion mixing is proceeded in compression mold, cover compressing tablet lid, set compressing tablet parameter, start compressing tablet.After compressing tablet completes, open mould, take out the sheet sample suppressing.To be checked.
(3.4), calibration criterion working curve: enter routine analyzer (name-Al
2o
3), by XRF setting parameter, sequentially determining Al-3#, Al-4#, Al-5#, Al-6#, above-mentioned six standard models of Al-7#, Al-8#, calibrate.
(3.5), measure testing sample: enter Al
2o
3routine analyzer, by XRF setting parameter, measures testing sample Al
2o
3, SiO
2content.
(4), result of calculation: this sample Al
2o
3content is 98.70%, SiO
2content is 0.033%.
Embodiment bis-
Measure Al in Al-Si Refractory Materials
2o
3, SiO
2the method of content, is characterised in that: with boric acid, be cementing agent, and pressed powder, Xray fluorescence spectrometer is measured.
Sheeter parameter
| Mixing ratio (boric acid+test portion) | Pressure (MPa) | Rise time (s) | Retention time (s) |
| (1:1) | 30 | 10 | 50 |
XRF instrument parameter
| Element | Spectral line | Crystal | Peak position/° | Detector | Tube current (mA) | Tube voltage (KV) |
| Al | Kα | PE002 | 144.745 | Flow | 160 | 25 |
| Si | Kα | PE002 | 108.972 | Flow | 160 | 25 |
(1) reagent, using in measuring process is as follows
(1.1), boric acid, top grade is pure, (after milling, 200 orders sieve, and put into exsiccator standby after oven dry)
(1.2), detector gas (P-10), 90% argon gas+10% methane
(1.3), aluminium oxide standard model GBW03115, national standard material (Al
2o
3=28.57%, SiO
2=55.90%)
(1.4), aluminium oxide standard model GSBD52001-92, national standard material (Al
2o
3=79.26%, SiO
2=1.49%)
(1.5), aluminium oxide standard model GSBD44001-92, national standard material (Al
2o
3=90.58%, SiO
2=4.20%)
(1.6), aluminium oxide standard model BY(A) 4-2#, national standard material (Al
2o
3=98.86%, SiO
2=0.012%)
(1.7), aluminium oxide standard model 418#, national standard material (Al
2o
3=87.16%, SiO
2=6.19%)
(1.8), aluminium oxide standard model 413#, national standard material (Al
2o
3=37.12%, SiO
2=44.02%)
(2), sampling: by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator.
(3), analysis experimental procedure is as follows:
(3.1), take test portion: accurately take sample 5.00g, be accurate to 0.01g.
(3.2), mix test portion: the sample of step (3.1) is transferred in mortar, takes 5.00g boric acid (1.1) and mix, grind and fully mix, treat compressing tablet.
(3.3), compressing tablet: open sheeter, the mixing test portion mixing is proceeded in compression mold, cover compressing tablet lid, set compressing tablet parameter, start compressing tablet.After compressing tablet completes, open mould, take out the sheet sample suppressing.To be checked.
(3.4), calibration criterion working curve: enter routine analyzer (name-Al
2o
3), by XRF setting parameter, sequentially determining Al-3#, Al-4#, Al-5#, Al-6#, above-mentioned six standard models of Al-7#, Al-8#, calibrate.
(3.5), measure testing sample: enter Al
2o
3routine analyzer, by XRF setting parameter, measures testing sample Al
2o
3, SiO
2content.
(4), result of calculation: this sample Al
2o
3content is 59.15%, SiO
2content is 33.18%.
Embodiment tri-
Measure Al in Al-Si Refractory Materials
2o
3, SiO
2the method of content, is characterised in that: with boric acid, be cementing agent, and pressed powder, Xray fluorescence spectrometer is measured.
Sheeter parameter
| Mixing ratio (boric acid+test portion) | Pressure (MPa) | Rise time (s) | Retention time (s) |
| (1:1) | 30 | 10 | 50 |
XRF instrument parameter
| Element | Spectral line | Crystal | Peak position/° | Detector | Tube current (mA) | Tube voltage (KV) |
| Al | Kα | PE002 | 144.745 | Flow | 160 | 25 |
| Si | Kα | PE002 | 108.972 | Flow | 160 | 25 |
(1) reagent, using in measuring process is as follows
(1.1), boric acid, top grade is pure, (after milling, 200 orders sieve, and put into exsiccator standby after oven dry)
(1.2), detector gas (P-10), 90% argon gas+10% methane
(1.3), aluminium oxide standard model GBW03115, national standard material (Al
2o
3=28.57%, SiO
2=55.90%)
(1.4), aluminium oxide standard model GSBD52001-92, national standard material (Al
2o
3=79.26%, SiO
2=1.49%)
(1.5), aluminium oxide standard model GSBD44001-92, national standard material (Al
2o
3=90.58%, SiO
2=4.20%)
(1.6), aluminium oxide standard model BY(A) 4-2#, national standard material (Al
2o
3=98.86%, SiO
2=0.012%)
(1.7), aluminium oxide standard model 418#, national standard material (Al
2o
3=87.16%, SiO
2=6.19%)
(1.8), aluminium oxide standard model 413#, national standard material (Al
2o
3=37.12%, SiO
2=44.02%)
(2), sampling: by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator.
(3), analysis experimental procedure is as follows:
(3.1), take test portion: accurately take sample 5.00g, be accurate to 0.01g.
(3.2), mix test portion: the sample of step (3.1) is transferred in mortar, takes 5.00g boric acid (1.1) and mix, grind and fully mix, treat compressing tablet.
(3.3), compressing tablet: open sheeter, the mixing test portion mixing is proceeded in compression mold, cover compressing tablet lid, set compressing tablet parameter, start compressing tablet.After compressing tablet completes, open mould, take out the sheet sample suppressing.To be checked.
(3.4), calibration criterion working curve: enter routine analyzer (name-Al
2o
3), by XRF setting parameter, sequentially determining Al-3#, Al-4#, Al-5#, Al-6#, above-mentioned six standard models of Al-7#, Al-8#, calibrate.
(3.5), measure testing sample: enter Al
2o
3routine analyzer, by XRF setting parameter, measures testing sample Al
2o
3, SiO
2content.
(4), result of calculation: this sample Al
2o
3content is 61.79%, SiO
2content is 21.30%.
Claims (4)
1. a method of measuring aluminium oxide and dioxide-containing silica in Al-Si Refractory Materials, is characterized in that: comprise the following steps:
-Criterion working curve:
1) prepare 4 above standard models, in described standard model, the shared weight ratio of aluminium oxide and silicon dioxide is different;
2) adopting boric acid is that cementing agent, working pressure machine carry out respectively pressed powder by standard model, makes standard model compressing tablet; The design parameter of pressed powder is as follows: boric acid and treat that the weight mixing ratio of compressing tablet sample is 1:1, and the compressing tablet pressure of pressing machine rises under 30 MPa the compressing tablet pressure at 30 MPa and keeps 50s at 10s;
3) use Xray fluorescence spectrometer, measure respectively the XRF characteristic spectral line intensity of above-mentioned standard model compressing tablet, the design parameter of XRF is as follows: while measuring element aluminum, adopt spectral line K α, crystal PE002,144.745 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; While measuring elemental silicon, adopt spectral line K α, crystal PE002,108.972 ° of peak positions, detector Flow, tube current 160 mA, tube voltage 25 KV; Then, XRF characteristic spectral line intensity and corresponding aluminium oxide and dioxide-containing silica are carried out to linear regression, obtain respectively the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity;
Aluminium oxide and the dioxide-containing silica of-mensuration sample to be tested:
4), by 200 order sieve for test portion to be measured, infrared lamp is dried 30min, puts into exsiccator stand-by;
5) use boric acid for cementing agent, test portion to be measured that step 4) is obtained are according to step 2) design parameter carry out pressed powder, make sample to be tested compressing tablet;
6) by the XRF setting parameter in step 3), use Xray fluorescence spectrometer to measure the XRF characteristic spectral line intensity of above-mentioned sample to be tested compressing tablet, and by the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity, read the content of aluminium oxide and silicon dioxide in testing sample.
2. the method for aluminium oxide and dioxide-containing silica in mensuration Al-Si Refractory Materials according to claim 1, it is characterized in that: described step 2) and 5) in boric acid be the pure boric acid of top grade, before use, after milling, after sieving, drying, to put into exsiccator standby for 200 orders.
3. the method for aluminium oxide and dioxide-containing silica in mensuration Al-Si Refractory Materials according to claim 1, it is characterized in that: described step 3) and 6) in the detector gas of Xray fluorescence spectrometer be P-10 gas, the argon gas by 90% and 10% methane blended gas form.
4. the method for aluminium oxide and dioxide-containing silica in mensuration Al-Si Refractory Materials according to claim 1, it is characterized in that: use 4 kinds of above national certified reference materials, carry out described step 2)～3) sample preparation and detect to analyze, continuous 9 tests, average, optimize the standard working curve of the corresponding XRF characteristic spectral line of aluminium oxide and silicon dioxide intensity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310703019.8A CN103674984A (en) | 2013-12-19 | 2013-12-19 | Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310703019.8A CN103674984A (en) | 2013-12-19 | 2013-12-19 | Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103674984A true CN103674984A (en) | 2014-03-26 |
Family
ID=50313189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310703019.8A Pending CN103674984A (en) | 2013-12-19 | 2013-12-19 | Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103674984A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104865285A (en) * | 2015-05-20 | 2015-08-26 | 中华人民共和国防城港出入境检验检疫局 | Method for rapidly determining aluminum species in dried beancurd sticks by adopting X-ray fluorescence spectrometer |
| CN105486706A (en) * | 2014-09-19 | 2016-04-13 | 鞍钢股份有限公司 | Method for measuring aluminum in aluminum wire |
| CN105866154A (en) * | 2016-03-31 | 2016-08-17 | 天津渤化永利化工股份有限公司 | Method for determining ferroalloy by using powder compressed tablet |
| CN108226202A (en) * | 2017-12-29 | 2018-06-29 | 黄河三角洲京博化工研究院有限公司 | A kind of method that dioxide-containing silica is measured using XRF Fluorescence Spectrometer |
| CN109070143A (en) * | 2016-01-20 | 2018-12-21 | 黑熊碳有限公司 | The method for sorting tire |
| CN109324074A (en) * | 2018-10-30 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content |
| CN111076991A (en) * | 2018-12-11 | 2020-04-28 | 广东特地陶瓷有限公司 | Preparation method and application of substrate for rapidly measuring external irradiation dose of ceramic tile |
| CN113447330A (en) * | 2021-06-30 | 2021-09-28 | 中国一冶集团有限公司 | Method for determining content of impurity components in white corundum by X-ray fluorescence spectrometry |
| CN114689632A (en) * | 2022-04-28 | 2022-07-01 | 中建材（蚌埠）光电材料有限公司 | Glass raw material tabletting method suitable for X-ray fluorescence spectrometer analysis |
| CN114778247A (en) * | 2022-04-26 | 2022-07-22 | 鞍钢集团矿业有限公司 | Preparation method of iron ore sample tablet for detection of fluorescence analyzer |
| CN115791860A (en) * | 2022-12-05 | 2023-03-14 | 山东国瓷功能材料股份有限公司 | Method for measuring copper and aluminum element contents, copper-aluminum ratio and silicon-aluminum ratio in molecular sieve |
| CN116183576A (en) * | 2022-12-09 | 2023-05-30 | 中国矿业大学 | Method for measuring content of free silicon dioxide in coal dust based on internal standard method |
| CN116990346A (en) * | 2023-09-27 | 2023-11-03 | 天津市贰拾壹站检测技术有限公司 | Method for measuring acidity coefficient of rock wool based on differential scanning calorimetry |
-
2013
- 2013-12-19 CN CN201310703019.8A patent/CN103674984A/en active Pending
Non-Patent Citations (8)
| Title |
|---|
| 丛秋兹: "《多晶二维X射线衍射》", 31 August 1997, 科学出版社 * |
| 曲月华等: "X射线荧光光谱法测定铝质耐火材料中主次成分", 《冶金分析》 * |
| 曹春娥等: "《无机材料测试技术》", 30 June 2011, 江西高校出版社 * |
| 朱卫华: "《大学化学实验 下册》", 31 January 2013, 科学出版社 * |
| 杨丽荣等: "铝硅质耐火材料的XRF分析法", 《鞍钢技术》 * |
| 杨明太等: "《实用X射线光谱分析》", 30 November 2008, 原子能出版社 * |
| 王亦军等: "《仪器分析实验》", 31 March 2009, 化学工业出版社 * |
| 苏作为: "X荧光分析仪在玻璃纤维原料检测中的应用", 《玻璃纤维》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486706A (en) * | 2014-09-19 | 2016-04-13 | 鞍钢股份有限公司 | Method for measuring aluminum in aluminum wire |
| CN104865285A (en) * | 2015-05-20 | 2015-08-26 | 中华人民共和国防城港出入境检验检疫局 | Method for rapidly determining aluminum species in dried beancurd sticks by adopting X-ray fluorescence spectrometer |
| CN109070143A (en) * | 2016-01-20 | 2018-12-21 | 黑熊碳有限公司 | The method for sorting tire |
| CN109070143B (en) * | 2016-01-20 | 2020-07-17 | 黑熊碳有限公司 | Method for sorting tires |
| CN105866154A (en) * | 2016-03-31 | 2016-08-17 | 天津渤化永利化工股份有限公司 | Method for determining ferroalloy by using powder compressed tablet |
| CN108226202A (en) * | 2017-12-29 | 2018-06-29 | 黄河三角洲京博化工研究院有限公司 | A kind of method that dioxide-containing silica is measured using XRF Fluorescence Spectrometer |
| CN109324074A (en) * | 2018-10-30 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content |
| CN111076991A (en) * | 2018-12-11 | 2020-04-28 | 广东特地陶瓷有限公司 | Preparation method and application of substrate for rapidly measuring external irradiation dose of ceramic tile |
| CN113447330A (en) * | 2021-06-30 | 2021-09-28 | 中国一冶集团有限公司 | Method for determining content of impurity components in white corundum by X-ray fluorescence spectrometry |
| CN114778247A (en) * | 2022-04-26 | 2022-07-22 | 鞍钢集团矿业有限公司 | Preparation method of iron ore sample tablet for detection of fluorescence analyzer |
| CN114689632A (en) * | 2022-04-28 | 2022-07-01 | 中建材（蚌埠）光电材料有限公司 | Glass raw material tabletting method suitable for X-ray fluorescence spectrometer analysis |
| CN115791860A (en) * | 2022-12-05 | 2023-03-14 | 山东国瓷功能材料股份有限公司 | Method for measuring copper and aluminum element contents, copper-aluminum ratio and silicon-aluminum ratio in molecular sieve |
| CN116183576A (en) * | 2022-12-09 | 2023-05-30 | 中国矿业大学 | Method for measuring content of free silicon dioxide in coal dust based on internal standard method |
| CN116183576B (en) * | 2022-12-09 | 2024-01-26 | 中国矿业大学 | Method for measuring content of free silicon dioxide in coal dust based on internal standard method |
| CN116990346A (en) * | 2023-09-27 | 2023-11-03 | 天津市贰拾壹站检测技术有限公司 | Method for measuring acidity coefficient of rock wool based on differential scanning calorimetry |
| CN116990346B (en) * | 2023-09-27 | 2023-12-26 | 天津市贰拾壹站检测技术有限公司 | Method for measuring acidity coefficient of rock wool based on differential scanning calorimetry |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103674984A (en) | Method for measuring content of aluminum oxide and silicon dioxide in aluminum-silicon fireproof material | |
| CN105241907B (en) | With the method for X-ray fluorescence spectra analysis pig iron composition | |
| CN103674985B (en) | A kind of accurately and reliably, silicon, sulfur, the detection method of P elements in simple and rapid steel-making exothermic mixture | |
| CN101526488A (en) | Method for analyzing components of iron ore by using X-ray fluorescence spectrum | |
| CN102269719B (en) | X-fluorescence film-pressing method for measuring content of components in ferric oxide powder | |
| CN102809578A (en) | Method of measuring component contents in fluorite by applying X fluorescence powder tablet pressing method | |
| CN109085136B (en) | Method for measuring content of oxide components in cement raw material by near-infrared diffuse reflection spectrum | |
| CN108802084A (en) | X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide | |
| CN106093002B (en) | Device and method that is a kind of while measuring sulfate radical and phosphate radical in high activity liquid waste | |
| CN103293175A (en) | Method for measuring chemical components of liquid sodium silicate | |
| CN108827993A (en) | Realize quickly measurement high performance magnetic material BMS-12 in lanthanum, calcium, cobalt each element content method | |
| CN101487796B (en) | Method for measuring melamine content in solid example | |
| CN104535600B (en) | The method of chrome green in wavelength dispersion X-ray fluorescence spectrometry measure stuffing sand | |
| CN108226202A (en) | A kind of method that dioxide-containing silica is measured using XRF Fluorescence Spectrometer | |
| CN106324006A (en) | Method for rapidly determining heavy metal element chromium in soil with X-ray fluorescent spectrometry | |
| CN106248708A (en) | A kind of X fluorescence spectrum method rapid assay methods to heavy metals in soil lead | |
| CN108195865A (en) | For the submerged arc welding flux standard sample and preparation method of X-ray fluorescence spectra analysis | |
| CN111751320A (en) | Method and system for detecting content of components in raw cement based on waveband selection | |
| CN105181726A (en) | Transmission-type X fluorescent device | |
| CN204630955U (en) | Plunderring into formula X-fluorescence measurement mechanism of a kind of quick detection Heavy Metals in Cosmetics content | |
| CN107907536A (en) | A kind of improved method of EDTA titration measurings calcium content | |
| CN106918610A (en) | Using TiO in X-ray fluorescence spectra analysis titanium dioxide2The method of content | |
| CN103353453A (en) | Inductively coupled plasma-atomic emission spectrometry (ICP-AES) method for testing chemical components of blue phosphors of plasma display panel (PDP) | |
| CN102095703A (en) | Method for carrying out near infrared spectrum non-destructive analysis on amoxicillin capsules | |
| CN212622330U (en) | Handheld metal spectrum analyzer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140326 |