WO2010004999A1 - 配合原料の水分測定方法及び水分測定装置 - Google Patents
配合原料の水分測定方法及び水分測定装置 Download PDFInfo
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- WO2010004999A1 WO2010004999A1 PCT/JP2009/062381 JP2009062381W WO2010004999A1 WO 2010004999 A1 WO2010004999 A1 WO 2010004999A1 JP 2009062381 W JP2009062381 W JP 2009062381W WO 2010004999 A1 WO2010004999 A1 WO 2010004999A1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 75
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/16—Sintering; Agglomerating
- C22B1/20—Sintering; Agglomerating in sintering machines with movable grates
- C22B1/205—Sintering; Agglomerating in sintering machines with movable grates regulation of the sintering process
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/16—Sintering; Agglomerating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/317—Special constructive features
- G01N2021/3174—Filter wheel
Definitions
- the present invention relates to a moisture measuring method and a moisture measuring device for blended raw materials.
- the present invention relates to a technique for measuring moisture in a sintered raw material obtained by blending a plurality of types of raw materials before blending using absorption of infrared water.
- sintering raw materials obtained by blending two or more brands of iron ore as raw materials and auxiliary raw materials such as powdered coke and limestone as fuel are sintered in a sintering machine.
- auxiliary raw materials such as powdered coke and limestone as fuel
- the iron ore and the auxiliary raw material before blending are referred to as a pre-blending raw material
- the raw material after blending is referred to as a blended raw material or a sintered raw material.
- the sintering process water is added to the sintering raw material in a mixer and mixed and granulated. Next, the granulated sintered raw material is charged in layers in a sintering machine, and the surface is ignited. The sintering machine sucks air from below the charged sintering raw material. Thereby, air passes toward the downward direction from the upper direction of a sintering raw material. Then, the sintering reaction proceeds gradually downward from the surface while the powder coke burns.
- the granulation of the sintering raw material is a process for producing pseudo particles of about 3 to 5 mm through the moisture contained in the sintering raw material.
- the pseudo particles have a structure in which fine particles having a particle size of 0.5 mm or less are mainly attached to core particles having a particle size of 1 mm or more.
- the granulation property of the sintering raw material greatly depends on the moisture content. For example, if there is not enough moisture, fine particles remain and the air permeability in the sintering machine deteriorates, resulting in a decrease in productivity. On the other hand, even if the water is excessive, the bonding force between the particles decreases, so that it is not possible to make particles having a target size.
- moisture management of the sintering raw material is particularly important in the granulation process of the sintering machine.
- it is necessary to measure the moisture content of the sintering raw material after granulation on the outlet side of the mixer. Then, the amount of water added is managed so that the measured moisture content of the sintered raw material becomes the target value.
- the moisture of iron ore sent from the raw material yard by a belt conveyor is not constant. For example, if there is rain when raw materials are stacked in the yard, the moisture content is different between the surface layer and the inside of the yard mountain. Therefore, it is desirable to constantly monitor the moisture content of the sintering material, and to change the amount of water added when the moisture content changes to keep the moisture content of the sintering material constant. Thereby, the air permeability in a sintering machine is maintained favorably, and stable operation and sintering quality can be ensured.
- the dry mass method is an accurate and reliable moisture measurement method.
- a sample of a sintering raw material is taken from a conveyance line, and the sample is completely dried by a dryer equipped with an atmosphere heating chamber and an infrared lamp.
- the moisture content which the sample of the sintering raw material contained was calculated
- the dry mass method requires an operation of sampling and a drying time (30 minutes to 2 hours), and the measurement is intermittent. There is also a problem that the time delay until the measurement value is obtained is extremely large.
- a moisture content measuring method using an infrared moisture meter as a method for measuring the moisture content of a measurement object online without collecting a sample of a sintering raw material.
- the surface of the object to be measured is irradiated with infrared rays and the reflected light is observed.
- infrared rays are absorbed according to the amount of moisture at a specific wavelength of infrared rays, and the spectral reflectance at that wavelength decreases.
- the moisture content of the object to be measured is measured.
- the three-wavelength infrared moisture meter In three-wavelength type infrared moisture meter wavelengths around 1.9 ⁇ m or 2.0 ⁇ m below as the absorption wavelength lambda W by water is used. Reference wavelengths ( ⁇ L , ⁇ S ) are respectively determined on the long wavelength side and the short wavelength side of the absorption wavelength ⁇ W by water. For the reference wavelengths ( ⁇ L , ⁇ S ), a wavelength that is as close as possible to the absorption wavelength ⁇ W and is not affected by moisture is selected.
- the reference spectral reflectance r W0e of the measurement object at the wavelength ⁇ W is calculated.
- the reference spectral reflectance of the measurement object, the object to be measured in the dry state is a calculated value assuming the spectral reflectance at a wavelength lambda W.
- w the moisture content of the measurement object (usually expressed in mass%).
- k the absorbance of the object to be measured.
- a and b are constants depending on the characteristics of the object to be measured. If the constants a and b corresponding to the object to be measured are inaccurate, an error occurs in the moisture measurement.
- the relationship between the water content w of the object to be measured and the infrared absorbance k due to the water varies depending on the type of the object to be measured.
- One reason is that the penetration depth of infrared rays varies depending on the substance.
- Another reason is that the amount of water near the surface of the object to be measured observed with infrared rays and the total amount of water contained in the object to be measured do not match due to the influence of water absorption or the like of the object to be measured.
- the infrared absorbance k C and the water content w C due to the water content are experimentally measured in advance for the sample of the object to be measured. Based on the measurement result, the relationship between the absorbance k and the water content w in the measurement object is determined as shown in equation (4).
- the relational expression between the absorbance k and the water content w is called a calibration curve.
- the relationship (calibration curve) between the moisture content w and the absorbance k of the sintered raw material Even if the constants a and b in the above equation (4) are experimentally determined in advance, the relationship between w and k changes due to subsequent changes in the composition of the sintering raw material. Therefore, in order to accurately measure the moisture content w of the sintering raw material using a three-wavelength infrared moisture meter, the measurement is performed while correcting the relationship between w and k, that is, the calibration curve in a timely manner based on actual measurements. Need to do.
- Patent Document 1 when measuring the moisture of powder with an infrared moisture meter outdoors, the measurement fluctuation due to the change in atmospheric humidity cannot be ignored. Therefore, Patent Document 1 discloses a method of measuring the atmospheric humidity in the measurement optical path using infrared rays and correcting the moisture measurement value using infrared rays according to the humidity measurement value. Specifically, the constant b in the above equation (4) is changed according to the humidity measurement value.
- Patent Document 2 discloses that in a method for measuring moisture content of a sintered ore raw material using an infrared moisture meter, the properties of the mixed raw material are slightly different each time the raw material composition is changed, so that the moisture meter is calibrated every time the composition is changed. . Specifically, a correction value is automatically calculated from the deviation between the target moisture value obtained from the moisture control device and the moisture indication value using a statistical method, and the moisture value drift (b in equation (4) above is changed). Is calibrated by zero drift operation.
- Patent Document 3 is a method for measuring moisture content of a sintered raw material using infrared rays. Every time the sintering raw material is mixed, precise moisture measurement is performed by an absolute dry-type moisture measuring means immediately after the change. Corresponds to the measured moisture value by infrared absorption. Then, a new calibration curve is calculated by performing linear regression using the measured values of the prescribed number of times. In the embodiment, the prescribed number of times is normally 5 to 6 times.
- the present invention quickly corrects the relationship between the absorbance k and the water content w (calibration curve) even when the raw material composition is changed in the measurement of the water content of the raw material using absorption by infrared water.
- An object of the present invention is to provide a moisture measuring method and a moisture measuring device capable of measuring the moisture content w of the blended raw material.
- the present invention employs the following means in order to solve the above problems.
- the water content measurement method of the blending raw material using the three-wavelength infrared moisture meter of the present invention is the wavelength ⁇ absorbed by water in the moisture content measuring method of the blending raw material using the three-wavelength infrared moisture meter.
- k A reference wavelength combination in which b of aw + b can be regarded as zero within the allowable measurement error range of the infrared moisture meter is used regardless of the blending ratio of the raw material before blending.
- a k 0 square sum average value which is a value obtained by dividing the square sum of the absorbance k 0 of each of the plurality of raw materials before mixing by the number of the raw materials before mixing, is calculated.
- a long wavelength side reference wavelength candidate ⁇ L ′ having a k 0 square sum average value of 0.001 or less among the plurality of long wavelength side reference wavelength candidates ⁇ L ′. and selecting as the lambda L; may be further provided with.
- the long wavelength side reference wavelength candidate ⁇ L ′ having the smallest k 0 square sum average value is set as the long wavelength side reference wavelength ⁇ L. You may choose.
- a step of measuring; k 0 square which is a value obtained by dividing the sum of squares of absorbance k 0 of each of the plurality of raw materials before mixing by the number of raw materials before mixing for each of the plurality of reference wavelength combination candidates Calculating a sum average value;
- the k 0 square sum average values and selecting as the reference wavelength combination of the reference wavelength combination candidates to be 0.001 or less; may further comprise a.
- the reference wavelength combination candidate having the smallest k 0 square sum average value among the plurality of reference wavelength combination candidates is the reference wavelength combination.
- the reference wavelength combination may be selected using a plurality of bandpass filters that pass a specific wavelength.
- the reference wavelength combination may be selected based on a result of continuous-wave infrared spectroscopy.
- the blended material is a sintered material; the wavelength ⁇ W absorbed by the water is 1.9 ⁇ m or more and 2.0 ⁇ m or less. Yes;
- the long wavelength side reference wavelength ⁇ L may be a wavelength selected from a wavelength range of 2.2 ⁇ m to 2.4 ⁇ m.
- the short wavelength side reference wavelength ⁇ S may be a wavelength selected from a wavelength range of 1.6 ⁇ m to 1.8 ⁇ m.
- the water content measuring apparatus for the blended raw material of the present invention includes a light source for irradiating the blended raw material with infrared rays; a detector for detecting the reflected light of the infrared; wavelength ⁇ W absorbed by water, and longer than ⁇ W
- a band-pass filter that transmits each of the three wavelengths of the long-wavelength side reference wavelength ⁇ L and the short-wavelength side reference wavelength ⁇ S shorter than ⁇ W ; and the infrared spectral reflectances r W , r L , and r S , respectively.
- the moisture content of the blended raw material was calculated.
- the short wavelength side wavelength ⁇ S may be a wavelength selected from a wavelength range of 1.6 ⁇ m to 1.8 ⁇ m.
- the method for measuring the moisture content of the blended material according to the present invention uses the moisture content measuring apparatus for the blended material described in (11) above, and previously measured the absorbance k C of the sample of the blended material using the dry mass method. Divide by the measured moisture content w C of the blended raw material sample to calculate the proportionality coefficient a, measure the absorbance k for any blended raw material, and divide the absorbance k by the proportional coefficient a to obtain the blended raw material. The moisture content w of is measured.
- the moisture content of the sample of the blended raw material is measured offline by dry mass method after changing the raw material blend.
- a calibration curve can be created from the measurement-containing water content w C and the infrared absorbance k C at the time when the measurement is performed only once. That is, the calibration curve can be corrected accurately and quickly. This makes it possible to continuously and accurately measure the water content w of the blended raw material by infrared measurement.
- a suitable long wavelength side reference wavelength ⁇ L can be selected.
- the optimum long wavelength side reference wavelength ⁇ L can be selected.
- a suitable reference wavelength combination can be selected.
- an optimal reference wavelength combination can be selected.
- a suitable reference wavelength can be selected with a simple configuration.
- a suitable reference wavelength can be accurately selected.
- the above inventions (8) and (9) when a sintered raw material is used as a blending raw material, the relationship between the absorbance k and the moisture content w of the sintered raw material is a linear expression that passes near the origin. Therefore, the same effect as the above (1) can be obtained.
- the moisture content of the sintered raw material can be measured accurately and quickly.
- rW0e and rW0a can be suitably matched by appropriately selecting the reference wavelengths ⁇ S and ⁇ L.
- “b becomes zero” means that even if b is regarded as zero, the influence is within the allowable error range in moisture measurement.
- the present embodiment will be described using a sintered raw material as an object to be measured, the applicable object of the present invention is not limited to the measurement of moisture content in the sintered raw material.
- the present invention can also be applied to, for example, a method for measuring the moisture content of a blended raw material obtained by blending a plurality of pre-blending raw materials.
- All of the infrared moisture meters that are currently used generally have a value of 1.96 ⁇ m as the water absorption wavelength ⁇ W , a value of 1.8 ⁇ m as the reference wavelength ⁇ S on the short wavelength side, and a reference wavelength ⁇ L on the long wavelength side A value of 2.1 ⁇ m is adopted.
- the absorbance k measured by the infrared moisture meter is compared with the moisture content w measured by the dry mass method for the same sample. .
- the standard spectral reflectance rW0e is calculated by the above equation (2)
- the absorbance k is calculated by the above equation (3).
- the blended sintering raw material is a blend of several types of these raw materials A, B, C, D, and when the moisture content of the sintered raw material after blending is measured with an infrared moisture meter, The relationship between the moisture content and the absorbance k measured with an infrared moisture meter changes both the slope a and the intercept value b depending on the blending conditions.
- the measurement of the moisture content w C by the dry mass method and the measurement of the absorbance k C by the infrared moisture meter are performed on two or more sintered raw material samples having different moisture contents. It is necessary to prepare two or more sets of measurement values. However, it is difficult to obtain such measurement values quickly.
- the spectral reflectance rW0a is measured for each of the raw materials A, B, and C before blending in a completely dried state. Specifically, measurement is performed using a FT-IR infrared spectrometer at a wavelength in a continuous infrared region (range of 1.6 ⁇ m or more and 2.4 ⁇ m or less). The results are shown in FIGS. 2A, 2B, and 2C.
- the spectral reflectance measured when the wavelength is 1.96 ⁇ m (that is, the absorption wavelength ⁇ W by water) is obtained.
- This spectral reflectance is the true spectral reflectance rW0a of each of the raw materials A, B, and C before blending in a dried state.
- the wavelength is 1.8 ⁇ m (that is, the short wavelength side reference wavelength ⁇ S )
- the wavelength is 2.1 ⁇ m (that is, the long wavelength side reference wavelength ⁇ L ).
- Spectral reflectances r S and r L measured at times are obtained.
- the raw material before blending has a formation spectrum (for example, an intrinsic spectral characteristic spectrum in the case of iron ore), so that the true spectral reflectance r W0a in the dry state is It can be seen that the reference spectral reflectance rW0e is deviated. In particular, the degree of deviation is large in the raw material B before blending. For this reason, it was found that the absorbance did not become zero even when the water content was zero.
- a formation spectrum for example, an intrinsic spectral characteristic spectrum in the case of iron ore
- the reference wavelength shorter wavelength side 1.8 .mu.m not fixed with the longer wavelength side 2.1 .mu.m, the true spectral reflectance of the material prior to blending the dry state r W0a and the reference spectral reflectance r W0e and is possible match
- the measurement accuracy of the infrared moisture meter can be improved by changing (resetting) the slope a of the calibration curve with the moisture measurement value w C of the raw material sample before blending obtained by the dry mass method being true. Can be increased. That is, since an accurate calibration curve can be obtained, the water content w of the blended material can be determined with high accuracy from the measured absorbance k of the blended material.
- the spectral reflectance rW0a and the reference spectral reflectance rW0e are matched as much as possible.
- the selection of the appropriate reference wavelength should be made with consideration given to almost all pre-combination raw materials, not to take into account specific pre-combination raw materials. Therefore, a suitable reference wavelength was searched for by the following method. Seven kinds (A to G) of brands of main raw materials used as sintering raw materials were selected as raw material samples. These pre-mixing raw material samples were dried to make the water content zero. The wavelength ⁇ W that is absorbed by the water was 1.96 ⁇ m.
- Candidates for reference wavelength ⁇ S on the short wavelength side were 1.6 ⁇ m, 1.7 ⁇ m, and 1.8 ⁇ m.
- Candidates of 2.1 ⁇ m, 2.2 ⁇ m, 2.3 ⁇ m, and 2.4 ⁇ m were used as reference wavelengths ⁇ L on the long wavelength side.
- spectral reflectances (r S and r L ) at the respective candidate wavelengths of ⁇ S and ⁇ L were measured.
- the absorbance k 0 of the sample of the raw material before blending according to the following formula (3) ′ was calculated.
- k 0 ⁇ ln (r W0a / r W0e ) (3) ′ Since the dry state is to substitute zero for w in the equation (4), k 0 is equal to b.
- the square of the absorbance k 0 of the raw material thus calculated was also calculated for each of the seven types.
- the sum (that is, the sum of squares) of the squares of the respective absorbance k 0 was calculated.
- a value obtained by dividing the square sum by the number of raw materials before blending was calculated.
- a suitable reference wavelength for a plurality of types of raw materials before blending is selected by evaluating the square sum of k 0 , but the present invention is not limited to such an evaluation method. Absent.
- a suitable reference wavelength may be selected by evaluating the sum of absolute values of k 0 , the sum of squares of k 0 , or the like.
- a suitable reference wavelength may be selected by calculating a sum of squares or the like with a weight according to the mixing ratio.
- the reference wavelength ⁇ L on the long wavelength side is in the range of 2.2 ⁇ m or more and 2.4 ⁇ m or less
- the square sum of k 0 is 0.001 or less. And can be held to very few levels.
- the reference wavelength ⁇ L on the long wavelength side is in the range of 2.2 ⁇ m or more and 2.4 ⁇ m or less
- the reference wavelength ⁇ S on the short wavelength side is any wavelength in the range of 1.6 ⁇ m or more and 1.8 ⁇ m or less. Even so, the mean square sum of k 0 can be reduced.
- the absorbance k 0 according to the above equation (3) ′ is shown. Both ⁇ W are 1.96 ⁇ m.
- sample names: ⁇ , ⁇ , ⁇ The raw material to be blended and the blending amount were changed, and three kinds of sintered raw materials (after blending) (sample names: ⁇ , ⁇ , ⁇ ) were prepared.
- samples of sintered raw materials were prepared in which the moisture content was varied from 0 to 7%.
- the moisture content w by dry mass method was evaluated.
- ⁇ W is 1.96 ⁇ m
- ⁇ S 1.8 ⁇ m
- ⁇ L 2.1 ⁇ m
- ⁇ S 1.7 ⁇ m
- ⁇ L 2.3 ⁇ m.
- the horizontal axis is the moisture content w evaluated by the dry mass method
- the vertical axis is the absorbance k obtained by infrared moisture measurement
- the sintered raw materials ⁇ , ⁇ , and ⁇ after mixing are compared.
- both the slope a and the intercept b of the relationship between the moisture content w and the absorbance k of the sintered raw material (after blending) vary depending on the type of the sintered raw material.
- the slope a changes, but the relationship between the moisture content and the absorbance passes through the origin in any of the sintering raw materials. Recognize.
- the water was removed by drying plurality of mixing before the raw material, respectively, water and the absorbance measured k 0 for each previous raw material formulation is removed, the square sum average absorbance k 0 of the plurality of formulation before the raw material was measured
- the infrared moisture measurement is performed by selecting the reference wavelengths ⁇ S and ⁇ L so that the mean square sum of k 0 becomes a small value when calculated, a plurality of raw materials before blending are blended as measurement targets. It can be seen that even when the sintered raw material is used, the relationship (calibration curve) between the absorbance k and the water content w is always on a straight line passing through the vicinity of the origin.
- b is in the vicinity of zero regardless of the composition, but strictly speaking, b is within 0 ⁇ 0.005. This uncertainty of 0.005 corresponds to an error of 0.2% in moisture measurement. Therefore, if the error allowed in moisture measurement is 0.2%, there is no practical problem even if b is regarded as zero. Thus, b being equal to or less than the allowable measurement error indicates that even if b is regarded as zero, the influence is within an error range allowed for moisture measurement.
- the absorbance k 0 When the absorbance k 0 is measured for a plurality of pre-combination raw materials from which moisture has been removed and ⁇ S and ⁇ L are selected such that the square sum of the absorbance k 0 is small, the square sum of the absorbance k 0 is 0. If ⁇ S and ⁇ L that are 001 or less are selected, the square sum average of the absorbance k 0 is 1 ⁇ 2 or less compared to the conventional case, and a highly accurate moisture measurement can be performed.
- ⁇ L has a greater influence on the moisture measurement accuracy of the sintered raw material.
- lambda using the values which have been conventionally used as S lambda L only to optimize may select lambda L of square sum average of the absorbance k 0 is reduced.
- the most preferable result can be obtained by selecting a reference wavelength combination having the smallest square sum of the absorbance k 0 .
- a plurality of ⁇ L , or a combination of a plurality of ⁇ S and ⁇ L , for a reference spectral reflection at a wavelength ⁇ W is used.
- calculating the rate r W0e it is necessary to determine the absorbance k 0 from r W0a and r W0e actually measured with respect dried preformulation material of the sample.
- the spectral reflectance at each ⁇ L and ⁇ S can be measured by using a bandpass filter of the wavelength.
- the bandpass filter a filter that passes infrared rays having a wavelength of ⁇ 0.05 ⁇ m can be used.
- infrared spectrometry result of the continuous wavelength the predetermined lambda L, spectral reflectance at lambda S r L, by reading the r S It is also possible to select an optimum ⁇ L or an optimum combination of ⁇ S and ⁇ L.
- an FT-IR spectrophotometer can be used.
- the wavelength of 2.2 ⁇ m or more and 2.4 ⁇ m or less is used as the reference wavelength ⁇ L on the long wavelength side.
- the reference wavelength ⁇ L is used as the reference wavelength ⁇ L on the long wavelength side.
- the reference spectral reflectance r W0e at wavelength ⁇ W is calculated from the above, the absorbance k of the sintered raw material is obtained from r W and r W0e, and the moisture content w C of the sintered raw material sample measured in advance by a dry mass method or the like a method of calculating the water content w of the sintering raw material from the relationship between the water content w and the absorbance k containing determined based on the absorbance k C (cali
- the moisture content w of the sintered raw material is determined from the relationship between the moisture content w C and the absorbance k determined based on the moisture content w C of the sample of the blended raw material measured in advance and the absorbance k C.
- the relationship between the water content w and the absorbance k passes through the vicinity of the origin, so that the moisture content of the sintered raw material can be calculated by dividing the absorbance k by the proportional coefficient a.
- the conventionally used ⁇ S may be used as it is, but ⁇ S is selected from a wavelength range of 1.6 ⁇ m to 1.8 ⁇ m.
- the wavelength to be used may be used.
- the moisture measuring apparatus 1 of the present invention for measuring the moisture content of a sintering raw material using absorption of infrared rays by water is more effective than the first infrared ray having a wavelength ⁇ W absorbed by water and the wavelength ⁇ W.
- a light source 2 that irradiates the sintering material with a second infrared ray having a long wavelength ⁇ L and a third infrared ray having a wavelength ⁇ S shorter than the wavelength ⁇ W , and reflected light of the first to third infrared rays ,
- a band-pass filter 4 that transmits infrared rays of three wavelengths of wavelength ⁇ W , wavelength ⁇ L , and wavelength ⁇ S , and an arithmetic device 5.
- Spectral reflectances r W , r L , and r S of the sintering raw material are the band pass filters of the wavelength ⁇ W absorbed by water, the reference wavelength ⁇ L on the long wavelength side, and the reference wavelength ⁇ S on the short wavelength side, respectively. 4 (4 w , 4 L , 4 S ), respectively.
- the absorption wavelength falling within the scope a wavelength 1.9 ⁇ m or 2.0 ⁇ m as lambda W is use, the wavelength to be selected from 2.2 ⁇ m or 2.4 ⁇ m or less in the wavelength range as the lambda L is used.
- the relationship between the water content w and the absorbance k passes through the vicinity of the origin in any sintered raw material 6.
- a band-pass filter selection device 7 using motor rotation can be used for selection of the three band-pass filters 4 (4 w , 4 L , 4 S ).
- the moisture measuring apparatus of the sintering material of the present invention may be to use a wavelength selected from 1.6 ⁇ m or 1.8 ⁇ m below as lambda S.
- the brand and blending ratio of the raw material before blending of the sintered raw material after blending are Even if it changes, the relationship between the absorbance k and the water content w in the infrared analysis is a linear expression that always passes near the origin.
- the relationship between the moisture content w and the absorbance k is: Since it passes through the vicinity of the origin, it is possible to calculate the moisture content of the sintered raw material by dividing the absorbance k by the proportional coefficient a. Therefore, for any sintered raw material, for example, for the sintered raw material charged into the sintering machine at a timing determined within one day, the absorbance k C is measured, and the moisture content w is determined by a dry mass method. If C is measured and the proportionality constant a is calculated by the equation (1), the measurement accuracy of the moisture measuring method and the moisture measuring device of the present invention can always be maintained accurately.
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Abstract
Description
本願は、2008年7月7日に、日本に出願された特願2008-176786号に基づき優先権を主張し、その内容をここに援用する。
a=k/w …(1)
rW0e=rS+(λW-λS)×(rL-rS)/(λL-λS) …(2)
k=-ln(rW/rW0e) …(3)
k=a×w+b …(4)
ここで、wは被測定対象物の含有水分量(通常、質量%で表示)である。kは被測定対象物の吸光度である。a、bは被測定物の特性に依存した定数である。被測定物に対応した定数a、bが不正確であると水分測定に誤差を生じる。
(1)本発明の、3波長式赤外線水分計を用いた配合原料の含有水分測定方法は、3波長式赤外線水分計を用いた配合原料の含有水分測定方法において、水により吸収される波長λWより長い長波長側参照波長λLと、前記波長λWより短い短波長側参照波長λSと、の参照波長組み合わせとして、前記配合原料の含有水分量wと吸光度kとの関係式k=aw+bのbが、前記配合前原料の配合比率によらず、前記赤外線水分計の許容測定誤差の範囲内でゼロと見なせる参照波長組み合わせを用いる。
(2)上記(1)に記載の配合原料の含有水分測定方法は、前記長波長側参照波長λLの候補である長波長側参照波長候補λL’を複数仮定する工程と;複数の前記長波長側参照波長候補λL’の各々を用いた場合ごとに、水分が除去された状態の前記複数の配合前原料各々の吸光度k0を測定する工程と;複数の前記長波長側参照波長候補λL’の各々を用いた場合ごとに、前記複数の配合前原料各々の前記吸光度k0の二乗和を前記配合前原料の個数で除した値である、k0二乗和平均値を計算する工程と;前記複数の長波長側参照波長候補λL’のうち、前記k0二乗和平均値が0.001以下になる長波長側参照波長候補λL’を、前記長波長側参照波長λLとして選択する工程と;を更に備えても良い。
(3)上記(2)に記載の配合原料の水分測定方法では、前記k0二乗和平均値が最も小さい値となる長波長側参照波長候補λL’を前記長波長側参照波長λLとして選択しても良い。
(4)上記(2)に記載の配合原料の水分測定方法は、前記長波長側参照波長λLの候補である長波長側参照波長候補λL’を複数仮定する工程と;前記短波長側参照波長λSの候補である短波長側参照波長候補λS’を複数仮定する工程と;複数の前記長波長側参照波長候補λL’と、複数の前記短波長側参照波長候補λS’と、を組み合わせた参照波長組み合わせ候補を複数仮定する工程と;複数の前記参照波長組み合わせ候補各々を用いた場合ごとに、水分が除去された状態の前記複数の配合前原料各々の吸光度k0を測定する工程と;複数の前記参照波長組み合わせ候補各々を用いた場合ごとに、前記複数の配合前原料各々の吸光度k0の二乗和を配合前原料の個数で除した値である、k0二乗和平均値を計算する工程と;前記複数の参照波長組み合わせ候補のうち、前記k0二乗和平均値が0.001以下になる参照波長組み合わせ候補を前記参照波長組み合わせとして選択する工程と;を更に備えても良い。
(5)上記(4)に記載の配合原料の水分測定方法では、前記複数の参照波長組み合わせ候補のうち、前記k0二乗和平均値が最も小さい値となる参照波長組み合わせ候補を前記参照波長組み合わせとして選択しても良い。
(6)上記(1)に記載の配合原料の水分測定方法では、前記参照波長組み合わせは、特定の波長を通すバンドパスフィルターを複数利用して選択されても良い。
(7)上記(1)に記載の配合原料の水分測定方法では、前記参照波長組み合わせは、連続波長の赤外線分光測定結果に基づき選択されても良い。
(8)上記(1)に記載の配合原料の水分測定方法では、前記配合原料は焼結原料であり;前記水により吸収される波長λWは、1.9μm以上2.0μm以下の波長であり;前記長波長側参照波長λLは、2.2μm以上2.4μm以下の波長範囲から選択される波長であっても良い。
(9)上記(1)に記載の配合原料の水分測定方法では、前記短波長側参照波長λSは、1.6μm以上1.8μm以下の波長範囲から選択される波長であっても良い。
(10)前記(1)に記載の配合原料の水分測定方法では、前記配合原料の試料の吸光度kCを測定する工程と;乾燥質量法によって前記配合原料の試料の含有水分量wCを測定する工程と;前記配合原料の試料の吸光度kCを、前記配合原料の試料の含有水分量wCで除算することで比例係数aを算出する工程と;前記配合原料の吸光度kを、前記比例係数aで除算することで前記配合原料の含有水分量を算出する工程と;を備えても良い。
(11)本発明の配合原料の水分測定装置は、赤外線を配合原料に照射する光源と;前記赤外線の反射光を検出する検出器と;水により吸収される波長λWと、λWより長い長波長側参照波長λLと、λWより短い短波長側参照波長λSと、の3波長それぞれを透過するバンドパスフィルターと;前記赤外線の分光反射率rW、rL、rSをそれぞれ算出し、前記分光反射率rLと前記分光反射率rSとから基準分光反射率rW0eを算出し、前記分光反射率rWと前記分光反射率rW0eとから前記配合原料の吸光度kを算出し、予め測定した配合原料の試料の含有水分量wCと吸光度kCとに基づき作成された、配合原料の含有水分量wと吸光度kとの関係から、前記配合原料の含有水分量を算出する演算部と;を有する、配合原料の水分測定装置であって、前記配合原料は焼結原料であり;前記水により吸収される波長λWは1.9μm以上2.0μm以下の波長であり;前記長波長側参照波長λLは2.2μm以上2.4μm以下の波長範囲から選択される波長である。
(12)上記(11)に記載の配合原料の水分測定装置では、前記短波長側波長λSは1.6μm以上1.8μm以下の波長範囲から選択される波長であっても良い。
(13)本発明の配合原料の水分測定方法は、上記(11)に記載の配合原料の水分測定装置を用い、予め測定した配合原料の試料の吸光度kCを、予め乾燥質量法を用いて測定した配合原料の試料の含有水分量wCで除算して比例係数aを算出し、任意の配合原料について吸光度kを測定し、前記吸光度kを前記比例係数aで除算することによって前記配合原料の含有水分量wを測定する。
上記(2)の発明によれば、好適な長波長側参照波長λLを選択出来る。
上記(3)の発明によれば、最適な長波長側参照波長λLを選択出来る。
上記(4)の発明によれば、好適な参照波長組み合わせを選択出来る。
上記(5)の発明によれば、最適な参照波長組み合わせを選択出来る。
上記(6)の発明によれば、簡単な構成で好適な参照波長を選択できる。
上記(7)の発明によれば、正確に好適な参照波長を選択出来る。
上記(8)、(9)の発明によれば、配合原料として焼結原料が用いられる際に、焼結原料の吸光度kと含有水分量wとの関係が原点近傍を通過する一次式となるため、上記(1)と同様の効果が得られる。
上記(10)の発明によれば、正確且つ迅速な焼結原料の含有水分測定が可能となる。
k=a×w …(5)
となる。即ち(4)式のbがゼロとなる。この場合、定めるべき定数がaひとつとなるので、原料配合変更後の焼結原料の試料に対して乾燥質量法水分測定を1回行えば定数aを定めることができる。そして、参照波長λS、λLを適切に選択することにより、rW0eとrW0aとを好適に一致させ得ることが明らかとなった。
尚、ここで言う「bがゼロになる」とは、bをゼロと見なしてもその影響が水分測定における許容誤差の範囲内であることを意味する。
k0=-ln(rW0a/rW0e) …(3)’
乾燥状態とは(4)式のwにゼロを代入することであるから、k0はbに等しい。
このような本発明の焼結原料の水分測定装置を用いることにより、いずれの焼結原料6でも含有水分量wと吸光度kとの関係は原点近傍を通過することとなる。3枚のバンドパスフィルター4(4w、4L、4S)の選択については、モーターの回転を用いたバンドパスフィルター選択装置7を用いることができる。
2 光源
3 検出器
4 バンドパスフィルター
5 演算装置
6 焼結原料
7 バンドパスフィルター選択装置
Claims (13)
- 3波長式赤外線水分計を用いた配合原料の含有水分測定方法において、
水により吸収される波長λWより長い長波長側参照波長λLと、前記波長λWより短い短波長側参照波長λSと、の参照波長組み合わせとして、前記配合原料の含有水分量wと吸光度kとの関係式k=aw+bのbが、前記配合前原料の配合比率によらず、前記赤外線水分計の許容測定誤差の範囲内でゼロと見なせる参照波長組み合わせを用いることを特徴とする、配合原料の水分測定方法。 - 前記長波長側参照波長λLの候補である長波長側参照波長候補λL’を複数仮定する工程と;
複数の前記長波長側参照波長候補λL’の各々を用いた場合ごとに、水分が除去された状態の前記複数の配合前原料各々の吸光度k0を測定する工程と;
複数の前記長波長側参照波長候補λL’の各々を用いた場合ごとに、前記複数の配合前原料各々の前記吸光度k0の二乗和を前記配合前原料の個数で除した値である、k0二乗和平均値を計算する工程と;
前記複数の長波長側参照波長候補λL’のうち、前記k0二乗和平均値が0.001以下になる長波長側参照波長候補λL’を、前記長波長側参照波長λLとして選択する工程と;
を更に備えることを特徴とする、請求項1に記載の配合原料の水分測定方法。
- 前記k0二乗和平均値が最も小さい値となる長波長側参照波長候補λL’を前記長波長側参照波長λLとして選択することを特徴とする請求項2に記載の配合原料の水分測定方法。
- 前記長波長側参照波長λLの候補である長波長側参照波長候補λL’を複数仮定する工程と;
前記短波長側参照波長λSの候補である短波長側参照波長候補λS’を複数仮定する工程と;
複数の前記長波長側参照波長候補λL’と、複数の前記短波長側参照波長候補λS’と、を組み合わせた参照波長組み合わせ候補を複数仮定する工程と;
複数の前記参照波長組み合わせ候補各々を用いた場合ごとに、水分が除去された状態の前記複数の配合前原料各々の吸光度k0を測定する工程と;
複数の前記参照波長組み合わせ候補各々を用いた場合ごとに、前記複数の配合前原料各々の吸光度k0の二乗和を配合前原料の個数で除した値である、k0二乗和平均値を計算する工程と;
前記複数の参照波長組み合わせ候補のうち、前記k0二乗和平均値が0.001以下になる参照波長組み合わせ候補を前記参照波長組み合わせとして選択する工程と; を更に備えることを特徴とする、請求項2に記載の配合原料の水分測定方法。
- 前記複数の参照波長組み合わせ候補のうち、前記k0二乗和平均値が最も小さい値となる参照波長組み合わせ候補を前記参照波長組み合わせとして選択することを特徴とする請求項4に記載の配合原料の水分測定方法。
- 前記参照波長組み合わせは、特定の波長を通すバンドパスフィルターを複数利用して選択されることを特徴とする請求項1に記載の配合原料の水分測定方法。
- 前記参照波長組み合わせは、連続波長の赤外線分光測定結果に基づき選択されることを特徴とする請求項1に記載の配合原料の水分測定方法。
- 前記配合原料は焼結原料であり;
前記水により吸収される波長λWは、1.9μm以上2.0μm以下の波長であり;
前記長波長側参照波長λLは、2.2μm以上2.4μm以下の波長範囲から選択される波長である;
ことを特徴とする請求項1に記載の配合原料の水分測定方法。 - 前記短波長側参照波長λSは、1.6μm以上1.8μm以下の波長範囲から選択される波長であることを特徴とする請求項8に記載の配合原料の水分測定方法。
- 前記配合原料の試料の吸光度kCを測定する工程と;
乾燥質量法によって前記配合原料の試料の含有水分量wCを測定する工程と;
前記配合原料の試料の吸光度kCを、前記配合原料の試料の含有水分量wCで除算することで比例係数aを算出する工程と;
前記配合原料の吸光度kを、前記比例係数aで除算することで前記配合原料の含有水分量wを算出する工程と;
を備えることを特徴とする請求項1に記載の配合原料の水分測定方法。 - 赤外線を配合原料に照射する光源と;
前記赤外線の反射光を検出する検出器と;
水により吸収される波長λWと、λWより長い長波長側参照波長λLと、λWより短い短波長側参照波長λSと、の3波長それぞれを透過するバンドパスフィルターと;
前記赤外線の分光反射率rW、rL、rSをそれぞれ算出し、前記分光反射率rLと前記分光反射率rSとから基準分光反射率rW0eを算出し、前記分光反射率rWと前記分光反射率rW0eとから前記配合原料の吸光度kを算出し、予め測定した配合原料の試料の含有水分量wCと吸光度kCとに基づき作成された、配合原料の含有水分量wと吸光度kとの関係から、前記配合原料の含有水分量wを算出する演算部と;
を有する、配合原料の水分測定装置であって、
前記配合原料は焼結原料であり;
前記水により吸収される波長λWは1.9μm以上2.0μm以下の波長であり;
前記長波長側参照波長λLは2.2μm以上2.4μm以下の波長範囲から選択される波長である;
ことを特徴とする配合原料の水分測定装置。 - 前記短波長側波長λSは1.6μm以上1.8μm以下の波長範囲から選択される波長であることを特徴とする請求項11に記載の配合原料の水分測定装置。
- 請求項11に記載の配合原料の水分測定装置を用い、
予め測定した配合原料の試料の吸光度kCを、予め乾燥質量法を用いて測定した配合原料の試料の含有水分量wCで除算して比例係数aを算出し、
任意の配合原料について吸光度kを測定し、前記吸光度kを前記比例係数aで除算することによって前記配合原料の含有水分量wを測定する
ことを特徴とする配合原料の水分測定方法。
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