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JP2009180665A - Optical path-length variable cell - Google Patents

Optical path-length variable cell Download PDF

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JP2009180665A
JP2009180665A JP2008021236A JP2008021236A JP2009180665A JP 2009180665 A JP2009180665 A JP 2009180665A JP 2008021236 A JP2008021236 A JP 2008021236A JP 2008021236 A JP2008021236 A JP 2008021236A JP 2009180665 A JP2009180665 A JP 2009180665A
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optical path
sample
path length
light
optical
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Takao Shimizu
孝雄 清水
Ryusuke Takigawa
隆介 瀧川
Tomohiro Honda
知宏 本田
Koki Takao
幸来 高尾
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Chino Corp
Fukuoka University
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Fukuoka University
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Abstract

【課題】簡易的な構成で、測定対象の試料の透過率又は屈折率に応じた所望の光路長に調節できる。
【解決手段】測定対象となる試料Mが収容される試料測定用空間11と、該試料測定用空間11の略中間位置に連通するように対向して形成された開口穴14とを備え、開口穴14における試料流路11との接続部分の内周面に、試料Mの透過率又は屈折率に応じて光路長を調節するための位置調節用雌ネジ部15が形成されたセル本体10と、測定光又は透過光が通過する透過部材20bが装入される外周面に位置調節用雌ネジ部15と螺合するための位置調節用雄ネジ部23が形成された保護部材20aとを備え、試料Mの透過率又は屈折率に応じた最適な光路長となるように、保護部材20aを回転により光路と同方向に移動させて光路長の調節を行う。
【選択図】図2
[PROBLEMS] To adjust a desired optical path length according to the transmittance or refractive index of a sample to be measured with a simple configuration.
A sample measurement space 11 in which a sample M to be measured is accommodated, and an opening hole 14 formed so as to communicate with a substantially middle position of the sample measurement space 11 are provided. A cell main body 10 having a position adjusting female screw portion 15 for adjusting the optical path length according to the transmittance or refractive index of the sample M formed on the inner peripheral surface of the connection portion of the hole 14 to the sample flow path 11; A protective member 20a having a male screw part 23 for position adjustment for screwing with the female screw part 15 for position adjustment on the outer peripheral surface into which the transmission member 20b through which measurement light or transmitted light passes is inserted. The optical path length is adjusted by moving the protective member 20a in the same direction as the optical path by rotation so that the optical path length according to the transmittance or refractive index of the sample M is obtained.
[Selection] Figure 2

Description

本発明は、光学的に試料の透過率又は屈折率を測定するために用いられ、試料中を透過する光の光路長の調節が可能な光路長可変セルに関するものである。   The present invention relates to an optical path length variable cell that is used for optically measuring the transmittance or refractive index of a sample and is capable of adjusting the optical path length of light transmitted through the sample.

従来より、試料溶液に光を照射し、その光が試料を通過する際、対象となる物質による光の吸収の程度、すなわち吸光度を測定することにより、その物質の濃度を定量的に分析する吸光度分析法が知られている。そして、対象となる物質の吸光度は、入射光の強度I0 と透過光の強度Iとの比の対数が吸光物質の厚さdに比例することを表すランベルトの法則と、溶液による光の吸光係数が濃度cに依存することを表すベールの法則とを合せたランベルト・ベールの法則(下記式1)を用いて測定している。 Conventionally, when a sample solution is irradiated with light, and the light passes through the sample, the degree of light absorption by the target substance, that is, the absorbance is measured to quantitatively analyze the concentration of the substance. Analytical methods are known. The absorbance of the target substance is determined by the Lambert law indicating that the logarithm of the ratio of the incident light intensity I 0 to the transmitted light intensity I is proportional to the thickness d of the light absorbing substance, and the light absorption by the solution. The measurement is performed using the Lambert-Beer law (equation 1 below) combined with the Beer law, which indicates that the coefficient depends on the concentration c.

log10(I0 /I)=εcd …(式1)
ここで、log10(I0 /I)を吸光度、cがモル濃度の場合のεをモル吸光係数とする。
log 10 (I 0 / I) = εcd (Formula 1)
Here, log 10 (I 0 / I) is the absorbance, and ε when c is the molar concentration is the molar extinction coefficient.

この測定方法を用いて対象となる物質の吸光度を測定する場合、試料溶液の濃度によって異なるため、得られる吸光度を適当な値にするために光路長の変更が必要となるが、光路長を変更する場合は測定器具の組み替えや部品の交換などを行わなければならず、作業が煩雑であった。そこで、このような手間を省くため、下記特許文献1に開示される光路長可変セルが開発されている。   When measuring the absorbance of a target substance using this measurement method, the optical path length needs to be changed in order to obtain an appropriate value for the resulting absorbance because it varies depending on the concentration of the sample solution. In order to do this, it was necessary to change the measuring instrument or replace parts, which was cumbersome. Therefore, in order to save such trouble, an optical path length variable cell disclosed in Patent Document 1 below has been developed.

図8は、排水や環境水のCOD(化学的酸素要求量)測定値を測定するCOD測定装置に用いられる光路長可変セルの断面図である。この光路長可変型セル201は、互いに平行に配置された透明平板からなる光入射窓202aと光出射窓202bをもち被測定液が収容され又は流通するセル本体203と、対をなす平面対204a,204bをもちセル本体203内に着脱可能に挿入される透明材質の光路長変更ブロック204とを備えている。その光路長変更ブロック204が有する平面対204a,204bから、いずれかの厚さの平面対を選択してセル内の光路に挿入することで、光路長を複数段階に変更することができる。本発明の光路長可変型セル201を使用した吸光度測定方法は、測定光の光路Xに対してセル本体203を固定し、光路長変更ブロック204を測定光の光路を横切る方向に移動させることにより複数の光路長での吸光度測定を可能としている。そして、測定された吸光度が上限吸光度以下であるか否かを判定し、測定された吸光度が上限吸光度より大きいと判定したときに、光路長が短くなる方向に光路長変更ブロック204を移動させるためのモータ205を制御して光路長を変更している。
特開2006−194775号公報
FIG. 8 is a cross-sectional view of a variable optical path length cell used in a COD measurement apparatus that measures COD (chemical oxygen demand) measurement values of wastewater and environmental water. This variable optical path length type cell 201 has a light incident window 202a and a light exit window 202b made of transparent flat plates arranged in parallel with each other, and a cell body 203 in which a liquid to be measured is accommodated or circulated, and a plane pair 204a that makes a pair. , 204b and a transparent optical path length changing block 204 that is detachably inserted into the cell body 203. By selecting a plane pair of any thickness from the plane pairs 204a and 204b of the optical path length changing block 204 and inserting it into the optical path in the cell, the optical path length can be changed in a plurality of stages. In the absorbance measurement method using the variable optical path length cell 201 of the present invention, the cell main body 203 is fixed with respect to the optical path X of the measurement light, and the optical path length changing block 204 is moved in a direction crossing the optical path of the measurement light. It is possible to measure absorbance at multiple optical path lengths. Then, it is determined whether or not the measured absorbance is equal to or lower than the upper limit absorbance, and when it is determined that the measured absorbance is larger than the upper limit absorbance, the optical path length changing block 204 is moved in a direction in which the optical path length is shortened. The optical path length is changed by controlling the motor 205.
JP 2006-194775 A

しかしながら、特許文献1に開示された光路長可変セルでは、光路長を可変するための駆動部(モータ205)を制御し、光路長変更ブロック204を移動させることで光路長を変更しているが、このような構成とすると光路長を変更するための構成部品が多くなって装置全体の構成が大掛かりになってしまうとともに、製造コストが嵩むという問題があった。   However, in the optical path length variable cell disclosed in Patent Document 1, the optical path length is changed by controlling the drive unit (motor 205) for changing the optical path length and moving the optical path length changing block 204. In such a configuration, there are problems that the number of components for changing the optical path length increases and the configuration of the entire apparatus becomes large, and the manufacturing cost increases.

そこで、本発明は上記問題点に鑑みてなされたものであり、簡易的な構成で所望の光路長に調節可能な光路長可変セルを提供することを目的とするものである。   The present invention has been made in view of the above problems, and an object thereof is to provide an optical path length variable cell that can be adjusted to a desired optical path length with a simple configuration.

上記した目的を達成するために、請求項1記載の光路長可変セルは、測定対象となる試料に測定光を投光する投光部と、前記測定光が前記試料を透過した透過光を受光する受光部と、該受光部で受光した前記透過光の強度に基づき前記試料の透過率又は屈折率を算出する演算部とを備えた光学的測定部を有する光学的測定装置に用いられる光路長可変セルにおいて、
前記試料の測定を行うために前記投光部と前記受光部との間の光路に形成される試料測定用空間と、該試料測定用空間の略中間位置に連通するように前記投光部と前記受光部とが対向して形成された開口穴とを有するセル本体と、
前記測定光又は前記透過光が通過する透過部材と、該透過部材が装入される保護部材とからなる光学窓と、
前記セル本体に対して前記保護部材を前記光路と同方向に移動させ、前記試料の透過率又は屈折率に応じた光路長に調節する光路長調節手段とを備えたことを特徴とする。
In order to achieve the above object, an optical path length variable cell according to claim 1 is provided with a light projecting unit for projecting measurement light onto a sample to be measured, and light transmitted through the sample. An optical path length used in an optical measurement device having an optical measurement unit, and a calculation unit that calculates the transmittance or refractive index of the sample based on the intensity of the transmitted light received by the light reception unit In variable cell,
A sample measuring space formed in an optical path between the light projecting unit and the light receiving unit for measuring the sample, and the light projecting unit so as to communicate with a substantially middle position of the sample measuring space; A cell body having an opening hole formed facing the light receiving portion;
An optical window comprising a transmission member through which the measurement light or the transmission light passes, and a protective member into which the transmission member is inserted;
An optical path length adjusting means is provided for adjusting the optical path length according to the transmittance or refractive index of the sample by moving the protection member in the same direction as the optical path with respect to the cell body.

請求項2記載の光路長可変セルは、請求項1記載の光路長可変セルにおいて、前記光路長調節手段は、前記セル本体の前記開口穴における前記試料測定用空間との接続部分の内周面に形成された位置調節用雌ネジ部と、
前記保護部材の外周面に形成され、前記位置調節用雌ネジ部と螺合するための位置調節用雄ネジ部とからなり、
前記保護部材を回転により前記光路と同方向に移動させて前記試料の透過率又は屈折率に応じた光路長に調節することを特徴とする。
The optical path length variable cell according to claim 2 is the optical path length variable cell according to claim 1, wherein the optical path length adjusting means is an inner peripheral surface of a connection portion of the cell body with the sample measurement space in the opening hole. A female screw part for position adjustment formed on
It is formed on the outer peripheral surface of the protective member, and consists of a male screw part for position adjustment for screwing with the female screw part for position adjustment,
The protective member is moved in the same direction as the optical path by rotation to be adjusted to an optical path length corresponding to the transmittance or refractive index of the sample.

請求項3記載の光路長可変セルは、請求項1又は2記載の光路長可変セルにおいて、ヒートポンプシステムを循環する冷媒に混入するオイルの循環率(OCR)を測定するオイル循環率測定装置に用いられ、
前記透過部材が少なくとも近赤外光を透過する光学材料で形成されるとともに、少なくとも前記セル本体及び前記保護部材が耐圧性及び耐食性を有する金属材料で形成されていることを特徴とする。
The variable optical path length cell according to claim 3 is used in the variable optical path length cell according to claim 1 or 2 for an oil circulation rate measuring device for measuring a circulation rate (OCR) of oil mixed in a refrigerant circulating in the heat pump system. And
The transmitting member is formed of an optical material that transmits at least near-infrared light, and at least the cell body and the protective member are formed of a metal material having pressure resistance and corrosion resistance.

本発明の光路長可変セルによれば、測定対象となる試料の透過率又は屈折率に応じて保護部材を光路と同方向に移動させて位置調節を行えるため、簡易的な構成で試料に合った最適な光路長に調節することができる。   According to the optical path length variable cell of the present invention, the position can be adjusted by moving the protective member in the same direction as the optical path in accordance with the transmittance or refractive index of the sample to be measured. The optimum optical path length can be adjusted.

また、例えばCO2 ヒートポンプシステムにおけるOCR測定のような高圧下での光学的測定においても、透過部材が耐圧性を有するサファイアガラスで、また少なくともセル本体、保護部材が耐圧性及び耐食性を有する金属材料で形成されているため、このような高圧条件下であっても高性能に光学的測定を行うことができる。 Also, for example, in optical measurement under high pressure such as OCR measurement in a CO 2 heat pump system, the transmissive member is a sapphire glass having pressure resistance, and at least the cell body and the protective member are metal materials having pressure resistance and corrosion resistance. Therefore, optical measurement can be performed with high performance even under such a high pressure condition.

以下、本発明を実施するための最良の形態について、添付した図面を参照しながら詳細に説明する。図1は本発明に係る光路長可変セルの概略を説明するための説明図であり、図2は同光路長可変セルにおける各部の構成を説明するための断面図であり、図3は同光路長可変セルの光路長を調節する際の調節方法を説明するための断面図であり、図4、図5は同光路長可変セルの取付手順を説明するための断面図であり、図6は同光路長可変セルが採用されるCO2 ヒートポンプシステムのシステム構成図であり、図7は同光路長可変セルにおける光路長調節手段の他の実施例を説明するための概略説明図である。 Hereinafter, the best mode for carrying out the present invention will be described in detail with reference to the accompanying drawings. FIG. 1 is an explanatory diagram for explaining the outline of an optical path length variable cell according to the present invention, FIG. 2 is a cross-sectional view for explaining the configuration of each part in the optical path length variable cell, and FIG. FIG. 4 is a cross-sectional view for explaining an adjustment method when adjusting the optical path length of the variable-length cell, and FIGS. 4 and 5 are cross-sectional views for explaining the mounting procedure of the variable-length cell. FIG. FIG. 7 is a system configuration diagram of a CO 2 heat pump system employing the same optical path length variable cell, and FIG. 7 is a schematic explanatory diagram for explaining another embodiment of the optical path length adjusting means in the optical path length variable cell.

なお、以下の記載では、本発明を実施するための最良の形態として、測定対象となる試料が光路長可変セル内を流れる場合について説明しているが、試料をセル内に収容した状態で透過率又は屈折率を測定することも可能である。また便宜上、透過率から吸光度を測定する場合について述べているが、これに限定されない。   In the following description, as the best mode for carrying out the present invention, the case where the sample to be measured flows in the optical path length variable cell is described. However, the sample is transmitted in a state where the sample is accommodated in the cell. It is also possible to measure the refractive index or the refractive index. For convenience, the case where the absorbance is measured from the transmittance is described, but the present invention is not limited to this.

図1に示すように、本例の光路長可変セル1を備える光学的測定装置2は、光路長可変セル1と試料Mを光学的に測定する光学的測定部3とが光学手段4を介して接続されて構成されている。この光学手段4は、光学的測定部3から照射された試料Mが吸収する波長の光(以下、測定光と記す)をセル内に導くための投光側光ファイバ4aと、投光側光ファイバ4aから照射された測定光が試料Mを透過したときの光(以下、透過光と記す)を受光して光学的測定部3に導くための受光側光ファイバ4bとで構成される。各ファイバ4a、4bの先端にはファイバコネクタを介して光学レンズ4c、4dがそれぞれ装着されており、この光学レンズ4c、4d(本例では投光側光ファイバ4aには光学レンズ4cが接続され、受光側光ファイバ4bには光学レンズ4dが接続される)が光路長可変セル1に装着されている。また、光路長可変セル1は、セル内に試料Mを流入するための試料導入管5と、吸光度の測定が終了した試料Mをセル内から排出するための試料排出管6が接続されている。   As shown in FIG. 1, the optical measuring apparatus 2 including the optical path length variable cell 1 of this example includes an optical path length variable cell 1 and an optical measuring unit 3 that optically measures a sample M via optical means 4. Connected and configured. The optical means 4 includes a light-projecting-side optical fiber 4a for guiding light having a wavelength absorbed by the sample M irradiated from the optical measuring section 3 (hereinafter referred to as measurement light) into the cell, and light-projecting-side light. The light receiving side optical fiber 4b for receiving the light (hereinafter referred to as transmitted light) when the measurement light irradiated from the fiber 4a passes through the sample M and guiding it to the optical measuring unit 3 is constituted. Optical lenses 4c and 4d are attached to the ends of the fibers 4a and 4b via fiber connectors, respectively. These optical lenses 4c and 4d (in this example, the optical lens 4c is connected to the light projecting side optical fiber 4a). The optical lens 4d is connected to the light receiving side optical fiber 4b). The optical path length variable cell 1 is connected to a sample introduction tube 5 for allowing the sample M to flow into the cell and a sample discharge tube 6 for discharging the sample M for which the absorbance measurement has been completed from the cell. .

光学的測定部3は、例えばハロゲンランプなどの光源で構成され光路長可変セル1内の試料Mに透過させる測定光を投光側光ファイバ4aを介して投光する投光部3aと、例えばフォトダイオード等の受光素子で構成され試料Mに対して照射された光を受光側光ファイバ4bを介して受光する受光部3bと、受光部3bで受光した透過光の強度に基づく電気信号から試料Mの吸光度を算出する演算部3cとを備えて構成される。光学的測定装置3は、測定対象となる試料Mに投光した測定光が試料Mを透過したときの透過光を受光し、この透過光の強度に基づく吸光度を測定している。   The optical measuring unit 3 is composed of a light source such as a halogen lamp, for example, and a light projecting unit 3a that projects the measurement light transmitted through the sample M in the optical path length variable cell 1 through the light projecting side optical fiber 4a. A light receiving unit 3b configured to receive light irradiated to the sample M, which is composed of a light receiving element such as a photodiode, through the light receiving side optical fiber 4b, and an electric signal based on the intensity of transmitted light received by the light receiving unit 3b. And an arithmetic unit 3c for calculating the absorbance of M. The optical measuring device 3 receives the transmitted light when the measurement light projected on the sample M to be measured passes through the sample M, and measures the absorbance based on the intensity of the transmitted light.

次に、図2を参照しながら、本例の光路長可変セル1の構成について説明する。光路長可変セル1は、セル本体10、光学窓20、支持部材30、押さえ部材40、蓋部材50とで構成される。以下、各構成について詳細に説明する。   Next, the configuration of the optical path length variable cell 1 of this example will be described with reference to FIG. The optical path length variable cell 1 includes a cell body 10, an optical window 20, a support member 30, a pressing member 40, and a lid member 50. Hereinafter, each configuration will be described in detail.

セル本体10は、例えばSUS(好ましくはSUS316)、真鍮、テフロン(登録商標)などの耐圧性及び/又は耐食性を有する材料からなり、測定対象となる試料Mを収容するための所定径を有する試料測定用空間11が形成されている。試料測定用空間11の一端(図中左側)には、試料Mをセル本体10内に導入するための導入側開口部12が、他端(図中右側)には試料Mをセル本体10から排出するための排出側開口部13が設けられ、この導入側開口部12には試料Mを導入する試料導入管5が、排出側開口部13には試料Mを排出する試料排出管6がそれぞれ配管接続される。   The cell body 10 is made of a material having pressure resistance and / or corrosion resistance such as SUS (preferably SUS316), brass, Teflon (registered trademark), and the like, and has a predetermined diameter for accommodating the sample M to be measured. A measurement space 11 is formed. An introduction side opening 12 for introducing the sample M into the cell body 10 is provided at one end (left side in the figure) of the sample measurement space 11, and the sample M is provided from the cell body 10 at the other end (right side in the figure). A discharge side opening 13 for discharging is provided, the sample introduction pipe 5 for introducing the sample M into the introduction side opening 12, and the sample discharge pipe 6 for discharging the sample M into the discharge side opening 13, respectively. Piping is connected.

また、試料測定用空間11の略中間位置に連通するように所定径を有する開口穴14(本例では図中上側の開口穴14を投光側開口穴14a、図中下側の開口穴14を受光側開口穴14bとする)が対向して形成され、この2つの開口穴14a、14bが光学的測定部3からの測定光や試料Mを透過した透過光が通過する光路として機能する。そして、投光側開口穴14aには、光学的測定部3からの測定光を投光する投光側光ファイバ4aが、受光側開口穴14bには試料Mを透過した透過光を受光する受光側光ファイバ4bがそれぞれ接続される。また、開口穴14における試料測定用空間11との接続部分の内周面には、後述する保護部材20aと螺合し、測定する試料Mの吸光度に応じて光路長を調節するための光路長調節手段としての位置調節用雌ネジ部15が形成されているとともに、開口穴14におけるファイバ接続部分の外周面には、蓋部材50を螺合するための蓋部材用ネジ部16が形成されている。   Further, an opening hole 14 having a predetermined diameter so as to communicate with a substantially intermediate position of the sample measurement space 11 (in this example, the upper opening hole 14 in the figure is a light-projecting side opening hole 14a, and the lower opening hole 14 in the figure is shown). Are formed opposite to each other, and the two opening holes 14a and 14b function as an optical path through which the measurement light from the optical measurement unit 3 and the transmitted light transmitted through the sample M pass. Then, the light projecting side opening hole 14a receives a light projecting side optical fiber 4a that projects the measurement light from the optical measuring unit 3, and the light receiving side opening hole 14b receives light transmitted through the sample M. The side optical fibers 4b are connected to each other. An optical path length for adjusting the optical path length according to the absorbance of the sample M to be measured is screwed onto the inner peripheral surface of the connection portion of the opening hole 14 with the sample measurement space 11 and a protective member 20a described later. A position adjusting female screw portion 15 as an adjusting means is formed, and a cap member screw portion 16 for screwing the cap member 50 is formed on the outer peripheral surface of the fiber connecting portion in the opening hole 14. Yes.

光学窓20は、例えばSUS(好ましくはSUS316)、真鍮、テフロン(登録商標)などの耐圧性及び/又は耐食性を有する材料からなり、外径は開口穴14に装入する装入部品として開口穴14と略同径を有し、内径は後述する透過部材20bが装入可能なように透過部材20bと略同径の収納部21が形成された略カップ形状を成す保護部材20aと、少なくとも近赤外光を透過する例えば耐圧性及び耐食性を有するサファイアガラスや耐食性を有する石英ガラスなどの光学材料からなり、保護部材20aに装入する装入部品として保護部材20aの収納部21と略同径を有する円板形状を成し、保護部材20aの装入位置調節が終了後に装入される透過部材20bとで構成される。また、保護部材20aの収納部21の閉塞側には、光を通過させるための光通過穴22が形成されている。さらに、保護部材20aにおける光通過穴22形成側の外周面には、開口穴14に形成された位置調節用雌ネジ部15と螺合するための光路長調節手段としての位置調節用雄ネジ部23が形成されている。また、保護部材20aの収納部21の開口端外周には、ピンや専用の治具などを差し込んで保護部材20aを回動させて着脱若しくは位置調節するための着脱用穴24が形成されている。すなわち、保護部材20aは、開口穴14に装入した後、開口穴14に形成された位置調節用雌ネジ部15と螺合することで装着される。   The optical window 20 is made of a material having pressure resistance and / or corrosion resistance, such as SUS (preferably SUS316), brass, Teflon (registered trademark), and the outer diameter is an opening hole as a charging part to be inserted into the opening hole 14. 14, the inner diameter is at least close to the protective member 20a having a substantially cup shape in which a storage portion 21 having the same diameter as that of the transmission member 20b is formed so that the transmission member 20b described later can be inserted. For example, it is made of an optical material such as sapphire glass having pressure resistance and corrosion resistance and quartz glass having corrosion resistance, which transmits infrared light. And a transparent member 20b that is inserted after adjustment of the insertion position of the protection member 20a is completed. A light passage hole 22 for allowing light to pass through is formed on the closed side of the storage portion 21 of the protection member 20a. Further, a position adjusting male screw portion as an optical path length adjusting means for screwing with the position adjusting female screw portion 15 formed in the opening hole 14 is formed on the outer peripheral surface of the protective member 20a on the light passing hole 22 forming side. 23 is formed. In addition, on the outer periphery of the opening end of the storage portion 21 of the protection member 20a, an attachment / detachment hole 24 is formed for inserting / detaching or adjusting the position of the protection member 20a by inserting a pin or a dedicated jig. . That is, the protective member 20 a is mounted by being screwed into the position adjusting female screw portion 15 formed in the opening hole 14 after being inserted into the opening hole 14.

ここで、図3を参照しながら、光学窓20の装着位置の調節方法について説明する。測定対象となる試料Mによって吸光度が異なるため、測定する試料Mに合せて光路長を調節する必要がある。そこで、図示のように、投光側開口穴14a又は受光側開口穴14bの少なくとも一方の保護部材20aを所定方向に回転させ、その装入位置を図中上下方向に調節することで、測定する試料Mに最適な光路長に調節することができる。   Here, a method for adjusting the mounting position of the optical window 20 will be described with reference to FIG. Since the absorbance varies depending on the sample M to be measured, it is necessary to adjust the optical path length according to the sample M to be measured. Therefore, as shown in the figure, measurement is performed by rotating at least one of the protective member 20a of the light-projecting-side opening hole 14a or the light-receiving-side opening hole 14b in a predetermined direction and adjusting the loading position in the vertical direction in the figure. It is possible to adjust the optical path length optimal for the sample M.

なお、保護部材20aの位置調節は、試料Mの流れを遮断しないように試料測定用空間11の中心位置(図2の一点鎖線)よりも開口穴14側に位置するように調節するとともに、測定誤差を極力抑えるようにするべく投光側開口穴14a、受光側開口穴14bからの移動距離を均等にすることが望ましい。また、保護部材20aの移動距離は、形成された位置調節用雄ネジ部23のピッチによって異なるため、予め位置調節用雄ネジ部23のピッチから一回転当たりの移動距離を割り出しておくことで、精密に光路長の間隔調節が可能となる。   The position of the protective member 20a is adjusted so that the flow of the sample M is not interrupted so as to be positioned closer to the opening hole 14 than the center position of the sample measurement space 11 (the one-dot chain line in FIG. 2). In order to suppress the error as much as possible, it is desirable to make the movement distances from the light projecting side opening hole 14a and the light receiving side opening hole 14b uniform. Further, since the moving distance of the protective member 20a varies depending on the pitch of the formed male screw portion 23 for position adjustment, by calculating the moving distance per rotation from the pitch of the male screw portion 23 for position adjustment in advance, It is possible to precisely adjust the optical path length.

支持部材30は、例えばSUS(好ましくはSUS316)、真鍮、テフロン(登録商標)などの耐圧性及び/又は耐食性を有する材料からなり、外径は開口穴14に装入する装入部品として開口穴14と略同径を有し、内径は投光側光ファイバ4a、受光側光ファイバ4bに接続される光学レンズ4c、4dを収納するための貫通穴31が形成された筒形状を成している。支持部材30は、開口穴14に装入された光学窓20を支持するように装入される。また、支持部材30の所定箇所における外周面には、シールして気密性を確保するためのO−リング32や、高圧力下において常用されるバックアップリング33が装着される溝部34、35が形成されており、透過部材20bとの接触部分に形成された溝部34にはO−リング32が、他方の溝部35には順にO−リング32、バックアップリング33が、それぞれ装着される。   The support member 30 is made of a material having pressure resistance and / or corrosion resistance such as SUS (preferably SUS316), brass, Teflon (registered trademark), and the outer diameter is an opening hole as a charging part to be inserted into the opening hole 14. 14, the inner diameter has a cylindrical shape in which a through hole 31 for accommodating the optical lenses 4c and 4d connected to the light projecting side optical fiber 4a and the light receiving side optical fiber 4b is formed. Yes. The support member 30 is inserted so as to support the optical window 20 inserted in the opening hole 14. Further, on the outer peripheral surface at a predetermined location of the support member 30, there are formed groove portions 34 and 35 in which an O-ring 32 for sealing and ensuring airtightness and a backup ring 33 which is normally used under high pressure are mounted. The O-ring 32 is attached to the groove 34 formed in the contact portion with the transmitting member 20b, and the O-ring 32 and the backup ring 33 are attached to the other groove 35 in this order.

押さえ部材40は、例えばSUS(好ましくはSUS316)、真鍮、テフロン(登録商標)などの耐圧性及び/又は耐食性を有する材料からなり、外径は開口穴14に装入する装入部品として開口穴14と略同径を有し、内径は貫通穴31と連通するように貫通穴31と同径の貫通穴41が形成された筒形状を成している。そして、支持部材30の貫通穴31と、押さえ部材40の貫通穴41とで、投光側光ファイバ4a、受光側光ファイバ4bに接続される光学レンズ4c、4dを収納するレンズ収納穴を構成している。押さえ部材40は、支持部材30を装入した後にセル本体10から支持部材30が外れないように押さえ付けるべく開口穴14に装入される。なお、貫通穴41の内面にはファイバコネクタを螺合するためのネジ部42が形成されている。   The holding member 40 is made of a material having pressure resistance and / or corrosion resistance such as SUS (preferably SUS316), brass, Teflon (registered trademark), and the outer diameter is an opening hole as a charging part to be inserted into the opening hole 14. 14 has a cylindrical shape in which a through hole 41 having the same diameter as the through hole 31 is formed so as to communicate with the through hole 31. The through hole 31 of the support member 30 and the through hole 41 of the pressing member 40 constitute a lens storage hole for storing the optical lenses 4c and 4d connected to the light projecting side optical fiber 4a and the light receiving side optical fiber 4b. is doing. The pressing member 40 is inserted into the opening hole 14 so as to be pressed so that the supporting member 30 is not detached from the cell body 10 after the supporting member 30 is inserted. A threaded portion 42 for screwing the fiber connector is formed on the inner surface of the through hole 41.

蓋部材50は、例えばSUS(好ましくはSUS316)、真鍮、テフロン(登録商標)などの耐圧性及び/又は耐食性を有する材料からなり、凹型の蓋形状を成している。また、蓋部材50の内周面には、セル本体10に形成された蓋部材用ネジ部16と螺合するためのネジ部51が形成されるとともに、蓋部材50の閉塞端側には光学レンズ4c、4dを装入するための装入穴52が形成されている。蓋部材50は、光学窓20、支持部材30、押さえ部材40を順に装入した後、これらを固定するべく開口穴14を塞ぐように螺合して装着される。   The lid member 50 is made of a material having pressure resistance and / or corrosion resistance such as SUS (preferably SUS316), brass, Teflon (registered trademark), and has a concave lid shape. In addition, a screw portion 51 is formed on the inner peripheral surface of the lid member 50 so as to be screwed with the screw portion 16 for the lid member formed in the cell body 10, and an optical end is provided on the closed end side of the lid member 50. An insertion hole 52 for inserting the lenses 4c and 4d is formed. After the optical window 20, the support member 30, and the pressing member 40 are sequentially inserted, the lid member 50 is screwed and attached so as to close the opening hole 14 in order to fix them.

次に、図4、5を参照しながら、上述した光路長可変セル1の取付手順について説明する。なお、本例の光路長可変セル1における投光側開口穴14aと受光側開口穴14bは、その構造や装入される部品及び装入する順番が同一であるため、ここでは受光側開口穴14bへの取付手順の説明を省略し、投光側開口穴14aの取付手順のみを説明する。   Next, an attachment procedure of the optical path length variable cell 1 described above will be described with reference to FIGS. The light projecting side opening hole 14a and the light receiving side opening hole 14b in the optical path length variable cell 1 of this example have the same structure, parts to be loaded, and the order of loading. Description of the attachment procedure to 14b is abbreviate | omitted, and only the attachment procedure of the light emission side opening hole 14a is demonstrated.

図4(a)に示すように、まず、投光側開口穴14aに保護部材20aを装入する。このとき、測定する試料Mの吸光度に応じた最適な光路長となるように、セル本体10に螺合した保護部材20aを所定方向に回転させながら上下移動させ、最適な光路長となる位置まで調節する。次に、保護部材20aの装入位置が決まると、図4(b)に示すように、透過部材20bを装入する。そして、図4(c)に示すように、溝部34にはO−リング32、溝部35にO−リング32、バックアップリング33を装着した支持部材30を投光側開口穴14aに装入する。   As shown in FIG. 4A, first, the protection member 20a is inserted into the light projecting side opening hole 14a. At this time, the protective member 20a screwed to the cell body 10 is moved up and down while rotating in a predetermined direction so that the optimum optical path length according to the absorbance of the sample M to be measured is reached, until the optimum optical path length is reached. Adjust. Next, when the insertion position of the protection member 20a is determined, the transmission member 20b is inserted as shown in FIG. Then, as shown in FIG. 4C, the support member 30 having the O-ring 32 in the groove 34, the O-ring 32 and the backup ring 33 in the groove 35 is inserted into the light projecting side opening hole 14a.

そして、図5(a)〜(c)に示すように、まず装入した支持部材30の押さえとなる押さえ部材40を支持部材30の上に装入した後、蓋部材50をセル本体10に螺合する。次に、光学レンズ4cを貫通穴41に装入し、最後に不図示のファイバコネクタを貫通穴41に設けたネジ部42に螺合することにより、光学レンズ4cに投光側光ファイバ4aを接続して、光路長可変セル1の取り付けが完了する。   Then, as shown in FIGS. 5A to 5C, first, after the pressing member 40 serving as a pressing member for the loaded support member 30 is loaded on the support member 30, the lid member 50 is attached to the cell body 10. Screw together. Next, the optical lens 4c is inserted into the through hole 41, and finally a fiber connector (not shown) is screwed into the screw portion 42 provided in the through hole 41, whereby the light projecting side optical fiber 4a is connected to the optical lens 4c. After connecting, the attachment of the optical path length variable cell 1 is completed.

次に、図6を参照しながら、上述した光路長可変セル1の採用例について具体的に説明する。ここでは、自然冷媒としてCO2 を利用したCO2 ヒートポンプシステム101において、試料MであるCO2 に混入したオイルのオイル量の指標であるオイル循環率(OCR)の測定に使用した例である。
なお、以下で使用する光路長可変セルでは、CO2 ヒートポンプシステムのような高圧条件下であってもOCR測定を可能とするため、透過部材20bが耐圧性及び耐食性を有するサファイアガラスで形成され、セル本体10、保護部材20a、支持部材30、押さえ部材40、蓋部材50のうち少なくともセル本体10及び保護部材20aが耐圧性及び耐食性を有する金属材料であるSUS316で形成されている。
Next, an example in which the above-described optical path length variable cell 1 is employed will be specifically described with reference to FIG. Here, in the CO 2 heat pump system 101 using CO 2 as a natural refrigerant, it is an example used for measuring an oil circulation rate (OCR) that is an index of the amount of oil mixed in CO 2 as the sample M.
In the optical path length variable cell used below, in order to enable OCR measurement even under high pressure conditions such as a CO 2 heat pump system, the transmission member 20b is formed of sapphire glass having pressure resistance and corrosion resistance, Of the cell body 10, the protection member 20a, the support member 30, the pressing member 40, and the lid member 50, at least the cell body 10 and the protection member 20a are formed of SUS316, which is a metal material having pressure resistance and corrosion resistance.

まず、CO2 ヒートポンプシステム101について説明すると、冷媒としてCO2 を使用し、熱交換して気化した冷媒(CO2 )を高圧蒸気冷媒(CO2 )にするための圧縮機102、高圧高温冷媒(CO2 )を高圧低温冷媒(CO2 )に冷却するガスクーラ103、冷却された冷媒液(CO2 )を絞り膨張させて低圧・低温の液体混合体(蒸発冷媒(CO2 ))にするための膨張弁104、膨張によって一部蒸発した湿り蒸気冷媒(CO2 )を熱交換によって蒸発させるための蒸発器105が、この順でオイル混入の冷媒(CO2 )が流れるように一つの循環系を形成して配管接続された構成である。そして、本例の光路長可変セル1は、ガスクーラ103と膨張弁104との間に配管接続されている。 First, the CO 2 heat pump system 101 will be described. The compressor 102, which uses CO 2 as a refrigerant, converts the refrigerant (CO 2 ) vaporized by heat exchange into a high-pressure vapor refrigerant (CO 2 ), a high-pressure high-temperature refrigerant ( A gas cooler 103 that cools CO 2 ) to a high-pressure low-temperature refrigerant (CO 2 ), and squeezes and expands the cooled refrigerant liquid (CO 2 ) to form a low-pressure / low-temperature liquid mixture (evaporated refrigerant (CO 2 )). An expansion valve 104 and an evaporator 105 for evaporating wet vapor refrigerant (CO 2 ) partially evaporated by expansion through heat exchange are arranged in one circulation system so that oil-mixed refrigerant (CO 2 ) flows in this order. It is the structure formed and connected by piping. The variable optical path length cell 1 of this example is connected by piping between the gas cooler 103 and the expansion valve 104.

上記のように配管接続された光路長可変セル1でOCRを測定した結果から検量線を作成するとN=32、R=0.99、σ=0.05%となった。これは、従来からの光路長固定型セルを用いて測定した測定結果から作成された検量線と比較しても遜色無く高性能に測定できることを示している。なお、ここでNは測定回数を、Rは相関係数を、σは標準偏差を表している。   When a calibration curve was created from the result of OCR measurement using the optical path length variable cell 1 connected by piping as described above, N = 32, R = 0.99, and σ = 0.05%. This shows that high-performance measurement can be performed without inferiority to a calibration curve created from measurement results measured using a conventional optical path length fixed cell. Here, N represents the number of measurements, R represents a correlation coefficient, and σ represents a standard deviation.

このように、上述した光路長可変セル1は、透過部材20bを装入する保護部材20aに測定対象となる試料Mに基づく光路長に調節するための位置調節用雄ネジ部23が形成され、測定する試料Mに基づき保護部材20aを所定方向に移動させて位置調節を行うことで、最適な光路長に調節することができる。   Thus, in the optical path length variable cell 1 described above, the position adjusting male screw portion 23 for adjusting the optical path length based on the sample M to be measured is formed in the protective member 20a in which the transmitting member 20b is inserted, By adjusting the position by moving the protective member 20a in a predetermined direction based on the sample M to be measured, the optical path length can be adjusted to the optimum.

また、CO2 ヒートポンプシステムにおけるOCR測定のような高圧下(約20Mpa)での光学的測定を行った場合であっても、透過部材20bを耐圧性及び耐食性を有するサファイアガラスで形成し、セル本体10、保護部材20a、支持部材30、押さえ部材40、蓋部材50のうち少なくともセル本体10及び保護部材20aを耐圧性及び耐食性を有する金属材料であるSUS316で形成しているため、このような高圧条件下であっても高性能に光学的測定を行うことができる。 In addition, even when optical measurement is performed under high pressure (about 20 Mpa) such as OCR measurement in a CO 2 heat pump system, the transmission member 20b is formed of sapphire glass having pressure resistance and corrosion resistance, and the cell body 10, at least the cell body 10 and the protection member 20a among the protection member 20a, the support member 30, the pressing member 40, and the lid member 50 are formed of SUS316, which is a metal material having pressure resistance and corrosion resistance. Even under conditions, optical measurement can be performed with high performance.

ところで、上述した形態では、図1、2において導入側開口部12を図中左側、排出側開口部13を図中右側、また投光側開口穴14aを図中上側、受光側開口穴14bを図中下側として説明したが、セル本体10において試料測定用空間11に対して開口穴14が対向する位置に形成されていれば、各部の形成位置は特に限定されない。   By the way, in the form mentioned above, in FIGS. 1 and 2, the introduction side opening 12 is the left side in the drawing, the discharge side opening 13 is the right side in the drawing, the light projecting side opening hole 14a is the upper side in the drawing, and the light receiving side opening hole 14b is. Although described as the lower side in the figure, the formation position of each part is not particularly limited as long as the opening hole 14 is formed in the cell body 10 so as to face the sample measurement space 11.

また、試料の透過率又は屈折率に応じて光路長を調節するための光路長調節手段を、セル本体10の開口穴14に形成された位置調節用雌ネジ部15と、保護部材20aに形成された位置調節用雄ネジ部23とで構成し、開口穴14に保護部材20aを螺合してねじ込むことで試料の透過率又は屈折率に応じた光路長に可変する構造で説明した。
しかし、この光路長調節手段は、例えば図7(a)に示すように、保護部材20aの外周面に所定間隔で係止溝25を刻み、この係止溝25を開口穴14の内面に設けた凸状の係止部材26で任意の装入位置に固定する構造や、また図7(b)に示すように、開口穴14の内面に所定間隔で係止溝28を刻み、この係止溝28に保護部材20aの外面に設けた凸状の係止部材27を係止する構成とすることも可能である。
このように、光路長を調節するべく保護部材20aを光路と同方向に移動可能な構成であれば特に限定されない。
Further, the optical path length adjusting means for adjusting the optical path length according to the transmittance or refractive index of the sample is formed in the position adjusting female screw portion 15 formed in the opening hole 14 of the cell body 10 and the protective member 20a. The position adjusting male screw portion 23 is used, and the structure in which the protective member 20a is screwed into the opening hole 14 and screwed into the optical path length according to the transmittance or refractive index of the sample has been described.
However, in this optical path length adjusting means, for example, as shown in FIG. 7A, a locking groove 25 is cut at a predetermined interval on the outer peripheral surface of the protective member 20a, and this locking groove 25 is provided on the inner surface of the opening hole 14. A structure that is fixed at an arbitrary insertion position by a convex locking member 26, or as shown in FIG. 7B, a locking groove 28 is cut at a predetermined interval on the inner surface of the opening hole 14, and this locking is performed. It is also possible to adopt a configuration in which a convex locking member 27 provided on the outer surface of the protective member 20a is locked in the groove 28.
Thus, there is no particular limitation as long as the protection member 20a can be moved in the same direction as the optical path so as to adjust the optical path length.

以上、本願発明における最良の形態について説明したが、この形態による記述及び図面により本発明が限定されることはない。すなわち、この形態に基づいて当業者等によりなされる他の形態、実施例及び運用技術等はすべて本発明の範疇に含まれることは勿論である。   As mentioned above, although the best form in this invention was demonstrated, this invention is not limited with the description and drawing by this form. That is, it is a matter of course that all other forms, examples, operation techniques, and the like made by those skilled in the art based on this form are included in the scope of the present invention.

本発明に係る光路長可変セルの概略を説明するための説明図である。It is explanatory drawing for demonstrating the outline of the optical path length variable cell which concerns on this invention. 同光路長可変セルにおける各部の構成を説明するための断面図である。It is sectional drawing for demonstrating the structure of each part in the same optical path length variable cell. 同光路長可変セルの光路長を調節する際の調節方法を説明するための断面図である。It is sectional drawing for demonstrating the adjustment method at the time of adjusting the optical path length of the same optical path length variable cell. (a)〜(c) 同光路長可変セルの取付手順を説明するための断面図である。(A)-(c) It is sectional drawing for demonstrating the attachment procedure of the optical path length variable cell. (a)〜(c) 同光路長可変セルの取付手順を説明するための断面図である。(A)-(c) It is sectional drawing for demonstrating the attachment procedure of the optical path length variable cell. 同光路長可変セルが採用されるCO2 ヒートポンプシステムのシステム構成図である。It is a system configuration diagram of a CO 2 heat pump system the optical path length varying cell is employed. (a)〜(b) 同光路長可変セルにおける光路長調節手段の他の実施例を説明するための概略説明図である。(A)-(b) It is a schematic explanatory drawing for demonstrating the other Example of the optical path length adjustment means in the same optical path length variable cell. 従来の光路長可変セルを説明するための概略構成図である。It is a schematic block diagram for demonstrating the conventional optical path length variable cell.

符号の説明Explanation of symbols

1 光路長可変セル
2 光学的測定装置
3 光学的測定部(3a 投光部、3b 受光部、3c 演算部)
4 光学手段(4a 投光側光ファイバ、4b 受光側光ファイバ、4c,4d 光学レンズ)
5 試料導入管
6 試料排出管
10 セル本体
11 試料測定用空間
12 導入側開口部
13 排出側開口部
14 開口穴(14a 投光側開口穴、14b 受光側開口穴)
15 位置調節用雌ネジ部
16 蓋部材用ネジ部
20 光学窓(20a 保護部材、20b 透過部材)
21 収納部
22 光通過穴
23 位置調節用雄ネジ部
24 着脱用穴
25 係止溝
26 係止部材
27 係止部材
28 係止溝
30 支持部材
31 貫通穴
32 O−リング
33 バックアップリング
34,35 溝部
40 押さえ部材
41 貫通穴
42 ネジ部
50 蓋部材
51 ネジ部
52 装入穴
101 CO2 ヒートポンプシステム
102 圧縮機
103 ガスクーラ
104 膨脹弁
105 蒸発器
DESCRIPTION OF SYMBOLS 1 Optical path length variable cell 2 Optical measuring apparatus 3 Optical measuring part (3a light projection part, 3b light receiving part, 3c calculating part)
4 Optical means (4a light emitting side optical fiber, 4b light receiving side optical fiber, 4c, 4d optical lens)
5 Sample introduction tube 6 Sample discharge tube 10 Cell body 11 Sample measurement space 12 Introduction side opening 13 Discharge side opening 14 Opening hole (14a light emitting side opening hole, 14b light receiving side opening hole)
15 Female screw part for position adjustment 16 Screw part for lid member 20 Optical window (20a protection member, 20b transmission member)
DESCRIPTION OF SYMBOLS 21 Storage part 22 Light passage hole 23 Position adjustment male screw part 24 Detachment hole 25 Locking groove 26 Locking member 27 Locking member 28 Locking groove 30 Support member 31 Through-hole 32 O-ring 33 Backup ring 34, 35 Groove part 40 Holding member 41 Through hole 42 Screw part 50 Lid member 51 Screw part 52 Insertion hole 101 CO 2 heat pump system 102 Compressor 103 Gas cooler 104 Expansion valve 105 Evaporator

Claims (3)

測定対象となる試料に測定光を投光する投光部と、前記測定光が前記試料を透過した透過光を受光する受光部と、該受光部で受光した前記透過光の強度に基づき前記試料の透過率又は屈折率を算出する演算部とを備えた光学的測定部を有する光学的測定装置に用いられる光路長可変セルにおいて、
前記試料の測定を行うために前記投光部と前記受光部との間の光路に形成される試料測定用空間と、該試料測定用空間の略中間位置に連通するように前記投光部と前記受光部とが対向して形成された開口穴とを有するセル本体と、
前記測定光又は前記透過光が通過する透過部材と、該透過部材が装入される保護部材とからなる光学窓と、
前記セル本体に対して前記保護部材を前記光路と同方向に移動させ、前記試料の透過率又は屈折率に応じた光路長に調節する光路長調節手段とを備えたことを特徴とする光路長可変セル。
A light projecting unit for projecting measurement light onto a sample to be measured, a light receiving unit for receiving transmitted light transmitted through the sample by the measurement light, and the sample based on the intensity of the transmitted light received by the light receiving unit In an optical path length variable cell used in an optical measurement device having an optical measurement unit with a calculation unit that calculates the transmittance or refractive index of
A sample measuring space formed in an optical path between the light projecting unit and the light receiving unit for measuring the sample, and the light projecting unit so as to communicate with a substantially middle position of the sample measuring space; A cell body having an opening hole formed facing the light receiving portion;
An optical window comprising a transmission member through which the measurement light or the transmission light passes, and a protective member into which the transmission member is inserted;
An optical path length comprising an optical path length adjusting means for adjusting the optical path length according to the transmittance or refractive index of the sample by moving the protective member in the same direction as the optical path with respect to the cell body. Variable cell.
前記光路長調節手段は、前記セル本体の前記開口穴における前記試料測定用空間との接続部分の内周面に形成された位置調節用雌ネジ部と、
前記保護部材の外周面に形成され、前記位置調節用雌ネジ部と螺合するための位置調節用雄ネジ部とからなり、
前記保護部材を回転により前記光路と同方向に移動させて前記試料の透過率又は屈折率に応じた光路長に調節することを特徴とする請求項1記載の光路長可変セル。
The optical path length adjusting means includes a position adjusting female thread portion formed on an inner peripheral surface of a connection portion with the sample measurement space in the opening hole of the cell body,
It is formed on the outer peripheral surface of the protective member, and consists of a male screw part for position adjustment for screwing with the female screw part for position adjustment,
2. The optical path length variable cell according to claim 1, wherein the protective member is moved in the same direction as the optical path by rotation to adjust the optical path length according to the transmittance or refractive index of the sample.
ヒートポンプシステムを循環する冷媒に混入するオイルの循環率を測定するオイル循環率測定装置に用いられ、
前記透過部材が少なくとも近赤外光を透過する光学材料で形成されるとともに、少なくとも前記セル本体及び前記保護部材が耐圧性及び耐食性を有する金属材料で形成されていることを特徴とする請求項1又は2記載の光路長可変セル。
Used in an oil circulation rate measuring device that measures the circulation rate of oil mixed in the refrigerant circulating in the heat pump system,
2. The transmissive member is formed of an optical material that transmits at least near-infrared light, and at least the cell body and the protective member are formed of a metal material having pressure resistance and corrosion resistance. Or the optical path length variable cell of 2.
JP2008021236A 2008-01-31 2008-01-31 Optical path-length variable cell Pending JP2009180665A (en)

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