JP2007248330A - Moisture content meter - Google Patents
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Abstract
Description
本発明は、膜厚変動やベースラインの上下変動の影響を受けずに水分率を測定できる水分率計に関するものである。 The present invention relates to a moisture content meter capable of measuring a moisture content without being affected by fluctuations in film thickness or vertical fluctuations in a baseline.
水分率計に関連する先行技術文献としては次のようなものがある。 Prior art documents related to the moisture content meter include the following.
図３は従来より一般に使用されている従来例の構成説明図である。
図において、赤外線光源１からの光は、光ファイバー２を通り、投光ユニット３のレンズ４を介して測定対象であるフィルムサンプル５に照射される。
フィルムサンプル５を透過した光は、受光ユニット６のレンズ７を介し、光ファイバー８を通過して、受光器９に入射される。
FIG. 3 is a diagram illustrating the configuration of a conventional example that is generally used.
In the figure, light from an infrared light source 1 passes through an optical fiber 2 and is irradiated onto a film sample 5 as a measurement target via a lens 4 of a light projecting unit 3.
The light transmitted through the film sample 5 passes through the optical fiber 8 through the lens 7 of the light receiving unit 6 and enters the light receiver 9.
図４は、図３の構成の装置で測定した、プラスチックフィルム５の近赤外吸収スペクトルの模式図である。
図４中、Ａは、フィルム５中に含有する水分に起因する吸収ピーク、Ｃはフィルム５そのものの成分（炭化水素基）に起因する吸収ピークである。
図４では、同じフィルム５で水分率の違うサンプルの複数のスペクトルを重ね書きしてある。
吸光度（透過率の対数）は光路中に含まれる当該成分量に比例する性質がある。
FIG. 4 is a schematic diagram of the near-infrared absorption spectrum of the plastic film 5 measured with the apparatus having the configuration shown in FIG.
In FIG. 4, A is an absorption peak due to moisture contained in the film 5, and C is an absorption peak due to a component (hydrocarbon group) of the film 5 itself.
In FIG. 4, a plurality of spectra of samples having the same film 5 and different moisture contents are overwritten.
Absorbance (logarithm of transmittance) has a property proportional to the amount of the component contained in the optical path.
図３従来例では、フィルム５中の水分を測定する際にはＡ部のピーク高さを、膜厚を測定する際にはＣ部の吸光度（ピーク高さ）を測定し、それぞれ検量線を作成して水分率と膜厚を測定していた。
また、ベースラインの変動（上下動、傾き）の影響を軽減するために、ピーク両脇の点を含めて３波長の吸光度を測定し（水分率であればＡ点、Ｂ点、Ｂ‘点）、適当な演算式、例えば２Ａ−Ｂ−Ｂ'で補正を行っていた。いわゆる、３波長方式である。
In the conventional example of FIG. 3, when measuring the moisture in the film 5, the peak height of the A part is measured, and when measuring the film thickness, the absorbance (peak height) of the C part is measured. The moisture content and film thickness were measured.
In addition, in order to reduce the influence of baseline fluctuations (vertical movement, inclination), the absorbance at three wavelengths including the points on both sides of the peak was measured (points A, B, and B ′ if moisture content) ), Correction was performed with an appropriate arithmetic expression, for example, 2ABB ′. This is a so-called three-wavelength method.
このような装置においては、以下の間題点がある。
水分率を測定する場合、膜厚変動や、光路に対するフィルムの角度変動（斜めに光が通る）などがあると、水分率が同じサンプルでも光路中に存在する水分量が変化し、指示が変動する。
３点の波数での吸光度情報しか使用していないため、フィルム表面の粗さやフィルム中の不純物などの影響で、ベースラインが高さや傾き以外の変動を受けた場合に指示が変動する。
Such an apparatus has the following problems.
When measuring the moisture content, if there are film thickness fluctuations or film angle fluctuations with respect to the optical path (light passes diagonally), the amount of moisture present in the optical path changes even for samples with the same moisture content, and the indication varies. To do.
Since only the absorbance information at three wave numbers is used, the instruction varies when the baseline is subjected to variations other than the height and inclination due to the roughness of the film surface and impurities in the film.
本発明の目的は、上記の課題を解決するもので、膜厚変動や、ベースラインの複雑な変動に対して影響を受けにくい水分率計を提供することにある。 An object of the present invention is to solve the above-described problems, and to provide a moisture meter that is less susceptible to film thickness fluctuations and complicated baseline fluctuations.
このような課題を達成するために、本発明では、請求項１の水分率計においては、
近赤外吸光スペクトルを測定して水分率を演算する水分率計において、あらかじめ測定対象自体の基準スペクトルを求めておき測定対象自体の測定スペクトルを前記基準スペクトルに合わせるように補正係数を求める補正係数演算手段と、この補正係数演算手段で求められた補正係数を用いて測定された水分のスペクトルを補正して水分率を演算する補正水分率演算手段とを具備したことを特徴とする。
In order to achieve such a problem, in the present invention, in the moisture content meter of claim 1,
In a moisture meter that calculates the moisture content by measuring the near-infrared absorption spectrum, a correction coefficient for obtaining a correction coefficient so that the reference spectrum of the measurement object itself is obtained in advance and the measurement spectrum of the measurement object itself is matched with the reference spectrum It is characterized by comprising a calculating means and a corrected moisture content calculating means for calculating a moisture content by correcting the moisture spectrum measured using the correction coefficient obtained by the correction coefficient calculating means.
本発明の請求項２の水分率計においては、請求項１記載の水分率計において、
前記補正係数演算手段は、補正後のスペクトルと基準スペクトルの差の二乗和が最小になるようにして前記補正係数を求めるようにしたことを特徴とする。
In the moisture content meter according to claim 2 of the present invention, in the moisture content meter according to claim 1,
The correction coefficient calculation means is characterized in that the correction coefficient is obtained so that the sum of squares of the difference between the corrected spectrum and the reference spectrum is minimized.
本発明の請求項３の水分率計においては、請求項１又は請求項２記載の水分率計において、
前記測定対象自体の測定スペクトルの測定値には前もって二次微分処理が行われたことを特徴とする。
In the moisture meter according to claim 3 of the present invention, in the moisture meter according to claim 1 or 2,
The measurement value of the measurement spectrum of the measurement object itself is preliminarily subjected to a second derivative process.
本発明の請求項４の水分率計においては、請求項１乃至請求項３の何れかに記載の水分率計において、
前記補正水分率演算手段は、水分率を演算する演算式として、多変量解析法で計算された演算式が用いられたことを特徴とする。
In the moisture meter according to claim 4 of the present invention, in the moisture meter according to any one of claims 1 to 3,
The corrected moisture content calculating means is characterized in that an arithmetic expression calculated by a multivariate analysis method is used as an arithmetic expression for calculating the moisture content.
本発明の請求項１によれば、次のような効果がある。
測定対象自体から補正係数を求めて、水分のスペクトルを補正するようにしたので、膜厚変動やベースラインの上下変動の影響を受けずに水分率を測定できる水分率計が得られる。
According to claim 1 of the present invention, there are the following effects.
Since the correction coefficient is obtained from the measurement object itself and the moisture spectrum is corrected, a moisture meter capable of measuring the moisture content without being affected by fluctuations in film thickness or vertical fluctuations in the baseline can be obtained.
本発明の請求項２によれば、次のような効果がある。
補正係数演算手段は、補正後のスペクトルと基準スペクトルの差の二乗和が最小になるようにして補正係数を求めるようにしたので、より正確な補正係数が求められる水分率計が得られる。
According to claim 2 of the present invention, there are the following effects.
Since the correction coefficient calculation means obtains the correction coefficient so that the sum of squares of the difference between the corrected spectrum and the reference spectrum is minimized, a moisture meter that can obtain a more accurate correction coefficient can be obtained.
本発明の請求項３によれば、次のような効果がある。
測定対象自体の測定スペクトルの測定値には、前もって二次微分処理が行われたので、ベースラインの上下動と傾きの影響が極めて少なく水分率を測定できる水分率計が得られる。
According to claim 3 of the present invention, there are the following effects.
Since the measurement value of the measurement spectrum of the measurement object itself has been subjected to second-order differential processing in advance, a moisture meter capable of measuring the moisture content is obtained with extremely little influence of vertical movement and inclination of the baseline.
本発明の請求項４によれば、次のような効果がある。
補正水分率演算手段は、水分率を演算する演算式として、多変量解析法で計算された演算式が用いられたので、測定対象自体の微妙な成分変化や周囲温度の変化等に由来する、ベースラインやスペクトル形状の複雑な変動の影響を最小にできる水分率計が得られる。
According to claim 4 of the present invention, there are the following effects.
Since the calculation formula calculated by the multivariate analysis method is used as the calculation formula for calculating the moisture content, the correction moisture rate calculation means is derived from a subtle component change of the measurement object itself, a change in the ambient temperature, etc. A moisture meter can be obtained that can minimize the effects of complex variations in baseline and spectral shape.
以下本発明を図面を用いて詳細に説明する。
図１は本発明の一実施例の要部構成説明図、図２は図１の動作説明図である。
図において、図３と同一記号の構成は同一機能を表す。
以下、図３との相違部分のみ説明する。
Hereinafter, the present invention will be described in detail with reference to the drawings.
FIG. 1 is a diagram illustrating the configuration of the main part of one embodiment of the present invention, and FIG. 2 is a diagram illustrating the operation of FIG.
In the figure, configurations with the same symbols as in FIG. 3 represent the same functions.
Only the difference from FIG. 3 will be described below.
図１において、受光器１０は、補正係数演算手段１１と補正水分率演算手段１２とを有する。
補正係数演算手段１１は、あらかじめ測定対象自体の基準スペクトルＡ１を求めておき、測定対象自体の測定スペクトルＡ２を、基準スペクトルＡ１に合わせるように補正係数を求める。
In FIG. 1, the optical receiver 10 includes a correction coefficient calculation unit 11 and a corrected moisture percentage calculation unit 12.
The correction coefficient calculation means 11 obtains a reference spectrum A1 of the measurement object itself in advance, and obtains a correction coefficient so that the measurement spectrum A2 of the measurement object itself matches the reference spectrum A1.
補正水分率演算手段１２は、補正係数演算手段１１で求められた補正係数を用いて測定された水分のスペクトルＡ３を補正して水分率を演算する。
この場合は、補正係数演算手段１１は、補正後のスペクトルと基準スペクトルＡ１の差の二乗和が最小になるようにして補正係数を求めるようにしている。
The corrected moisture content calculating means 12 calculates the moisture content by correcting the moisture spectrum A3 measured using the correction coefficient obtained by the correction coefficient calculating means 11.
In this case, the correction coefficient calculation means 11 obtains the correction coefficient so that the sum of squares of the difference between the corrected spectrum and the reference spectrum A1 is minimized.
また、測定対象自体の測定スペクトルの測定値Ａ２には、前もって二次微分処理が行われている。
また、補正水分率演算手段１２は、水分率を演算する演算式として、多変量解析法で計算された演算式が用いられている。
In addition, the second derivative process is performed in advance on the measurement value A2 of the measurement spectrum of the measurement object itself.
The corrected moisture content calculating means 12 uses an arithmetic expression calculated by the multivariate analysis method as an arithmetic expression for calculating the moisture content.
具体的には、水分等の測定対象成分の吸収波数領域（図２中のＢ−Ａ−Ｂ‘）およびフィルムの主成分である炭化水素の吸収波数領域（図２中のＤ−Ｃ−Ｂ)の両方の領域を含む波数領域のスペクトルを測定する。
この段階で、必要に応じて、二次微分処理等の前処理を行い、ベースライン変動の影響等を極力取り除いても良い。
次に、フィルム主成分の吸収ピーク（図２中のＤ−Ｃ−Ｂ）の形状と大きさが、基準となるスペクトルに極力一致するように、スペクトル全体の補正を行う。
Specifically, the absorption wave number region of the component to be measured such as moisture (B-A-B 'in FIG. 2) and the absorption wave number region of the hydrocarbon that is the main component of the film (D-C-B in FIG. 2). ) Measure the spectrum in the wavenumber region including both regions.
At this stage, if necessary, pre-processing such as second-order differential processing may be performed to eliminate the influence of baseline fluctuations as much as possible.
Next, the entire spectrum is corrected so that the shape and size of the absorption peak (D-C-B in FIG. 2) of the main component of the film matches the reference spectrum as much as possible.
測定したスペクトル（図２中の細線）をａ（ｉ）、補正後のスペクトルをａ’（ｉ）、基準スペクトルをＡ（ｉ）とする。（ｉは吸光度を測定する波数点に対応する添え字）
ａ’（ｉ）＝ｂ×ａ（ｉ）＋ｃ （ｂ、ｃは定数） （式１）
で表せると仮定し、
The measured spectrum (thin line in FIG. 2) is a (i), the corrected spectrum is a ′ (i), and the reference spectrum is A (i). (I is a subscript corresponding to the wave number point at which absorbance is measured)
a ′ (i) = b × a (i) + c (b and c are constants) (Formula 1)
Assuming that
補正後のスペクトルと基準スペクトルのフィルム主成分の波数範囲での残差Ｄ〜Ｂ
Ｄ〜Ｂ＝Σ｛ａ’（ｉ）−Ａ（ｉ）｝２ （式２）
が最小になる条件で、定数ｂ、ｃを求め、それから補正スペクトルａ’（ｉ）を求める。たとえば、補正前のスペクトル（図中細線）を、基準スペクトル（図中太線）とほぼ一致した形状（図中太線）となる。
Residuals D to B in the wave number range of the film main component of the corrected spectrum and the reference spectrum
D to B = Σ {a ′ (i) −A (i)} 2 (Formula 2)
The constants b and c are obtained under the condition that becomes minimum, and then the corrected spectrum a ′ (i) is obtained. For example, the spectrum (thin line in the figure) before correction has a shape (thick line in the figure) that substantially matches the reference spectrum (thick line in the figure).
上記の処理で、定数ｃはベースライン変動の影響、定数ｂは膜厚変動の影響をキャンセルする効果を有する。
基準スペクトルＡ１の範囲に水分の吸収ピークを含めないことにより、水分率そのものが変動した際に、膜厚補正の効果に誤差を生じることを防いでいる。
In the above processing, the constant c has the effect of canceling the influence of the baseline fluctuation, and the constant b has the effect of canceling the influence of the film thickness fluctuation.
By not including the moisture absorption peak in the range of the reference spectrum A1, it is possible to prevent an error in the effect of the film thickness correction when the moisture content itself fluctuates.
すなわち、これらの前処理により、当該サンプルを、膜厚や表面の散乱状態が一定の理想的な形状に加工してスペクトルを測定したのと同等のスペクトルを得ることができる。 たとえば基準スペクトルを、膜厚１ｍｍ、表面がなめらかな状態のサンプルのスペクトルにしておけば良い。 That is, by these pretreatments, a spectrum equivalent to that obtained by processing the sample into an ideal shape having a constant film thickness and surface scattering state and measuring the spectrum can be obtained. For example, the reference spectrum may be a spectrum of a sample having a thickness of 1 mm and a smooth surface.
測定スペクトルから水分率を計算するには、多変量解析法、たとえばＰＬＳ法（部分最小二乗法）を用いる。
すなわち、上記前処理を実施した水分率が既知のサンプルのスペクトルを複数本用意しておき、複数の波数での吸光度（または吸光度を微分した値）の線形結合Ｂ〜Ｂ’
In order to calculate the moisture content from the measurement spectrum, a multivariate analysis method such as a PLS method (partial least square method) is used.
That is, a plurality of spectra of samples having a known moisture content subjected to the above pretreatment are prepared, and linear combinations B to B ′ of absorbances (or values obtained by differentiating absorbances) at a plurality of wave numbers.
Ｂ〜Ｂ’＝Σｄ（ｉ）×ａ’（ｉ）＋ｄ０ （式３）
で水分率が表せると仮定し、残差、すなわち（上式で計算した水分率値−真の水分率値）の二乗和が最小になるように、特定のアルゴリズムで係数ｄ（ｉ）、ｄ０をあらかじめ求めておき、水分率未知の（前処理後）スペクトルを式３に当てはめることにより、未知サンプルの水分率を求めることができる。
B to B ′ = Σd (i) × a ′ (i) + d0 (Formula 3)
Assuming that the moisture content can be expressed by a specific algorithm, the coefficients d (i) and d0 are determined so that the residual, that is, the sum of squares of the (moisture content value calculated by the above equation−true water content value) is minimized. Is obtained in advance, and the moisture content of the unknown sample can be obtained by applying the unknown (after pretreatment) spectrum to Equation 3.
各種前処理を行い、波数として多数の（例えば５０点）吸光度データを用いているため、ベースラインが複雑に曲がった形状に変化したりしても、影響を最小にするように検量線を作成することができる。
なお、この場合は、測定対象が炭化水素を主成分とする合成樹脂フィルムであり、測定対象自体の吸収波数域にＣＨ基の第１倍音である５７５０ｃｍ−１を含み、水分の吸収波数域に、ＯＨ基の結合音である５２００ｃｍ−１を含む。
Performs various pre-treatments and uses a large number of absorbance data (eg 50 points) as the wave number, so a calibration curve is created to minimize the impact even if the baseline changes to a complicated curved shape. can do.
In this case, the measurement target is a synthetic resin film containing hydrocarbon as a main component, the measurement target itself includes 5750 cm −1 , which is the first overtone of the CH group, in the absorption wave number range of moisture, , And 5200 cm −1 which is a bond sound of OH group.
この結果、
測定対象自体から補正係数を求めて、水分のスペクトルを補正するようにしたので、膜厚変動やベースラインの上下変動の影響を受けずに水分率を測定できる水分率計が得られる。
As a result,
Since the correction coefficient is obtained from the measurement object itself and the moisture spectrum is corrected, a moisture meter capable of measuring the moisture content without being affected by fluctuations in film thickness or vertical fluctuations in the baseline can be obtained.
補正係数演算手段１１は、補正後のスペクトルと基準スペクトルの差の二乗和が最小になるようにして補正係数を求めるようにしたので、より正確な補正係数が求められる水分率計が得られる。 Since the correction coefficient calculation means 11 obtains the correction coefficient so that the sum of squares of the difference between the corrected spectrum and the reference spectrum is minimized, a moisture meter capable of obtaining a more accurate correction coefficient can be obtained.
測定対象自体の測定スペクトルの測定値には、前もって二次微分処理が行われたので、ベースラインの上下動と傾きの影響が極めて少なく水分率を測定できる水分率計が得られる。 Since the measurement value of the measurement spectrum of the measurement object itself has been subjected to second-order differential processing in advance, a moisture meter capable of measuring the moisture content is obtained with extremely little influence of vertical movement and inclination of the baseline.
補正水分率演算手段１２は、水分率を演算する演算式として、多変量解析法で計算された演算式が用いられたので、測定対象自体の微妙な成分変化や周囲温度の変化等に由来する、ベースラインやスペクトル形状の複雑な変動の影響を最小にできる水分率計が得られる。 Since the arithmetic expression calculated by the multivariate analysis method is used as the arithmetic expression for calculating the moisture ratio, the corrected moisture percentage calculating means 12 is derived from a subtle component change of the measurement object itself, a change in ambient temperature, and the like. A moisture meter can be obtained that can minimize the effects of complex variations in baseline and spectral shape.
なお、以上の説明は、本発明の説明および例示を目的として特定の好適な実施例を示したに過ぎない。
したがって本発明は、上記実施例に限定されることなく、その本質から逸脱しない範囲で更に多くの変更、変形をも含むものである。
The above description merely shows a specific preferred embodiment for the purpose of explanation and illustration of the present invention.
Therefore, the present invention is not limited to the above-described embodiments, and includes many changes and modifications without departing from the essence thereof.
１ 赤外線光源
２ 光ファイバー
３ 投光ユニット
４ レンズ
５ フィルムサンプル
６ 受光ユニット
７ レンズ
８ 光ファイバー
９ 受光器
１０ 受光器
１１ 補正係数演算手段
１２ 補正水分率演算手段
Ａ１ 基準スペクトル
Ａ２ 測定対象自体の測定スペクトル
Ａ３ 水分のスペクトル
DESCRIPTION OF SYMBOLS 1 Infrared light source 2 Optical fiber 3 Light projection unit 4 Lens 5 Film sample 6 Light reception unit 7 Lens 8 Optical fiber 9 Light receiver 10 Light receiver 11 Correction coefficient calculation means 12 Correction moisture rate calculation means A1 Reference spectrum A2 Measurement spectrum of measurement object itself A3 Water content Spectrum of
Claims (4)
あらかじめ測定対象自体の基準スペクトルを求めておき測定対象自体の測定スペクトルを前記基準スペクトルに合わせるように補正係数を求める補正係数演算手段と、
この補正係数演算手段で求められた補正係数を用いて測定された水分のスペクトルを補正して水分率を演算する補正水分率演算手段と
を具備したことを特徴とする水分率計。 In a moisture meter that calculates the moisture content by measuring the near infrared absorption spectrum,
A correction coefficient calculating means for obtaining a correction coefficient so as to obtain a reference spectrum of the measurement object in advance and align the measurement spectrum of the measurement object itself with the reference spectrum;
A moisture content meter comprising: a corrected moisture content computing means for computing a moisture content by correcting a moisture spectrum measured using the correction coefficient obtained by the compensation coefficient computing means.
を特徴とする請求項１記載の水分率計。 The moisture content meter according to claim 1, wherein the correction coefficient calculation means obtains the correction coefficient so that the sum of squares of the difference between the corrected spectrum and the reference spectrum is minimized.
を特徴とする請求項１又は請求項２記載の水分率計。 The moisture content meter according to claim 1 or 2, wherein a second derivative process is performed in advance on the measurement value of the measurement spectrum of the measurement object itself.
を特徴とする請求項１乃至請求項３の何れかに記載の水分率計。
The moisture according to any one of claims 1 to 3, wherein the corrected moisture content calculating means uses an arithmetic expression calculated by a multivariate analysis method as an arithmetic expression for calculating the moisture content. Rate meter.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2006073860A JP2007248330A (en) | 2006-03-17 | 2006-03-17 | Moisture content meter |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2006073860A JP2007248330A (en) | 2006-03-17 | 2006-03-17 | Moisture content meter |
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| JP2007248330A true JP2007248330A (en) | 2007-09-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011069812A (en) * | 2009-08-31 | 2011-04-07 | Mitsui Chemicals Inc | Measuring method, method for manufacturing solar cell module, measuring device, the solar cell module, and evaluation method of the solar cell module |
| JP2011169704A (en) * | 2010-02-17 | 2011-09-01 | Shimadzu Corp | Data processor and program for the same |
| CN106767687A (en) * | 2017-02-22 | 2017-05-31 | 河海大学 | A kind of method of utilization remote sensing moisture measurement beach elevation |
-
2006
- 2006-03-17 JP JP2006073860A patent/JP2007248330A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011069812A (en) * | 2009-08-31 | 2011-04-07 | Mitsui Chemicals Inc | Measuring method, method for manufacturing solar cell module, measuring device, the solar cell module, and evaluation method of the solar cell module |
| JP2011169704A (en) * | 2010-02-17 | 2011-09-01 | Shimadzu Corp | Data processor and program for the same |
| CN106767687A (en) * | 2017-02-22 | 2017-05-31 | 河海大学 | A kind of method of utilization remote sensing moisture measurement beach elevation |
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