JP3422725B2 - An analyzer that simultaneously performs Raman spectroscopy and particle size distribution measurement - Google Patents

An analyzer that simultaneously performs Raman spectroscopy and particle size distribution measurement

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Publication number
JP3422725B2
JP3422725B2 JP13804999A JP13804999A JP3422725B2 JP 3422725 B2 JP3422725 B2 JP 3422725B2 JP 13804999 A JP13804999 A JP 13804999A JP 13804999 A JP13804999 A JP 13804999A JP 3422725 B2 JP3422725 B2 JP 3422725B2
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JP
Japan
Prior art keywords
particle size
size distribution
sample
raman
analyzer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
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JP13804999A
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Japanese (ja)
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JP2000329682A (en
Inventor
司 佐竹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Horiba Ltd
Original Assignee
Horiba Ltd
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Publication of JP2000329682A publication Critical patent/JP2000329682A/en
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Description

【発明の詳細な説明】 【0001】 【発明の属する技術分野】本発明は、ラマン分光分析と
粒度分布測定を同時に行う分析装置に関する。 【0002】 【従来の技術】試料の同定や定量分析を行うための装置
の1つにラマン分光分析器がある。従来のラマン分光分
析器では、レーザー光(単色光)を試料に照射し、生じ
たラマン散乱光のラマン・スペクトルを用いることで試
料の分析を行っている。 【0003】また、試料の粒度分布を測定するには、粒
度分布測定器が用いられている。従来の粒度分布測定器
では、レーザー光(単色光に限るものではない)を試料
に照射し、生じた散乱光および透過光を用いることで試
料の粒度分布測定を行っている。 【0004】そして、ある試料について、物質の同定や
定量分析とともに粒度分布の測定を行う必要がある場合
には、ラマン分光分析器と粒度分布測定器の両方を用
い、試料を一方の装置で測定した後に、他方の装置に搬
送して測定を行うようにしていた。 【0005】 【発明が解決しようとする課題】しかし、上記の構成で
は、試料を搬送することから測定に時間がかかり、ま
た、この時間の経過や試料の搬送によって、試料の性状
が変化する場合があり、迅速で、かつ正確な分析を行う
ことができなかった。 【0006】本発明は上述の事柄に留意してなされたも
ので、その目的は、同一試料の同一部分に対して、ラマ
ン分光分析および粒度分布測定を同時に、正確に、かつ
迅速に行うことが可能なラマン分光分析と粒度分布測定
を同時に行う分析装置を提供することである。 【0007】 【課題を解決するための手段】上記目的を達成するため
に、本発明のラマン分光分析と粒度分布測定を同時に行
う分析装置は、レーザー光源から試料に向けてレーザー
光を照射し、生じたラマン散乱光のラマン・スペクトル
を用いることで試料の同定および定量分析を行うラマン
分光分析器と、前記レーザー光照射により生じた散乱光
および透過光を用いて粒度分布を測定する粒度分布測定
器とよりなり、前記レーザー光源をラマン分光分析と粒
度分布測定に併用した。 【0008】上記の構成により、同一試料の同一部分に
対して、ラマン分光分析および粒度分布測定を同時に、
正確に、かつ迅速に行うことが可能なラマン分光分析と
粒度分布測定を同時に行う分析装置を提供することがで
きる。 【0009】 【発明の実施の形態】以下、本発明のラマン分光分析と
粒度分布測定を同時に行う分析装置の構成を図を用いて
説明する。図1は、本発明の一実施例に係るラマン分光
分析と粒度分布測定を同時に行う分析装置Dの構成を概
略的に示す図である。ラマン分光分析と粒度分布測定を
同時に行う分析装置Dは、試料Sが内部に貯留された試
料セル1と、試料セル1の一側に設けられたラマン分光
分析器Rおよび他側に設けられた粒度分布測定器Pとか
ら構成されている。 【0010】前記ラマン分光分析器Rは、レーザー光源
2から試料Sにレーザー光を照射して、生じたラマン散
乱光のラマン・スペクトルを用いることで試料Sの同定
および定量分析を行うものである。以下にその構成を示
す。 【0011】前記ラマン分光分析器Rの上流には、レー
ザー光源2が設けられている。このレーザー光源2は、
単色光からなるレーザー光(例えば633nmのHe−
Neレーザー)を照射するものである。このレーザー光
源2から照射されたレーザー光は、レーザー光源2の下
流側に設けられたレンズ3、反射鏡4、ビームスプリッ
タ5、レンズ6を順に経て、試料セル1に至るように構
成されている。 【0012】前記レンズ6を経たレーザー光は、試料S
の焦点位置Fに照射されるように構成されている。そし
て、前記焦点位置Fに前記レーザー光が照射されること
により、ラマン散乱光とレイリー散乱光とを含む散乱光
が生じ、生じた散乱光の一部が再びレンズ6、ビームス
プリッタ5を経て、ノッチフィルター7を通り、分光器
8に至る。 【0013】前記ノッチフィルター7は、横軸および縦
軸にそれぞれ周波数および散乱光強度をとった図1の拡
大図に示すグラフのように、強度の大きいレイリー散乱
光αを除去するためのものである。そのため、ノッチフ
ィルター7を経て分光器8に至るのはラマン散乱光のみ
となる。 【0014】前記分光器8は、光センサー9(例えばチ
ャージカップルドデバイス)を有しており、また、下流
側にはCPU10、表示部11がこの順に接続されてい
る。 【0015】前記表示部11では、例えば、横軸に周波
数、縦軸に散乱光強度がとられたグラフが表示され、得
られたラマン散乱光のラマン・スペクトルを視覚的に認
識することができる。また、このラマン・スペクトルを
用いることで、試料Sの同定および定量分析を行うこと
ができ、また、試料Sの濃度情報を得ることができる。 【0016】一方、前記粒度分布測定器Pは、ラマン分
光分析器Rのレーザー光源2から試料Sに照射されたレ
ーザー光によって生じた散乱光および透過光を用いて、
試料Sの粒度分布を測定するためのものである。以下に
その構成を示す。 【0017】前記ラマン分光分析器Rのレーザー光源2
からのレーザー光が、試料Sの前記焦点位置Fに照射さ
れて、透過光および散乱光が生じる。この透過光および
散乱光の一部は、試料セル1の下流に設けられた集光レ
ンズ12を経て、フォトダイオードからなる光検出器1
3に至る。 【0018】光検出器13の下流側には、光検出器13
からの信号を取り込むマルチプレクサ14、マルチプレ
クサ14からの信号が入力され、散乱光強度パターンに
基づいて演算を行って粒度分布を求めるためのCPU1
5、CPU15で求めた粒度分布を表示するための表示
部16が順に接続されている。 【0019】前記表示部16では、例えば、横軸に粒径
を、縦軸に頻度をとったグラフが表示され、測定して得
られた粒度分布を視覚的に認識することができる。 【0020】上記の構成からなるラマン分光分析と粒度
分布測定を同時に行う分析装置Dによって、同一試料の
同一位置における同時計測が可能となり、迅速に複数の
手法による分析を実現することができる。 【0021】上記の構成からなるラマン分光分析と粒度
分布測定を同時に行う分析装置Dにおいて、前記ラマン
分光分析器Rと前記粒度分布測定器Pを適宜に接続し
て、互いの測定結果を反映しあうようにすれば、ラマン
分析による濃度情報を粒度分布演算に反映することで、
粒度分布測定の信頼性を向上させることができ、また、
粒度分布測定の結果をラマン分光分析の微量分析に反映
することで、ラマン分析を用いた微量分析の信頼性を向
上させることができる。もちろん、両者の測定系の異常
判別なども簡単に行うことができる。 【0022】なお、上記の構成において、試料セル1は
試料Sを貯留するものに限らず、例えば試料Sを内部に
流通させる流通型のものでもよいし、内部に試料Sが流
れる配管の一部に、適宜の光を透過する窓を設けて、上
記流通側の試料セルと同様の機能を有するように構成し
たものでもよい。このように構成すれば、流通状態にあ
る試料も、ラマン分光分析と粒度分布測定を同時に行う
分析装置Dを用いて上記と同様の分析を行うことができ
る。 【0023】また、上記の構成において、試料Sの焦点
位置Fに対して前記ラマン分光分析器Rからレーザー光
を照射する方向および生じたラマン散乱光を受光する方
向と、前記粒度分布測定器Pが前記透過光および散乱光
の一部を受光する方向とが全て一直線上となるように設
けてもよいが、本発明のラマン分光分析と粒度分布測定
を同時に行う分析装置Dにおける光学的な配置はこれに
限るものではなく、例えば、試料Sの焦点位置Fに対し
て前記ラマン分光分析器Rからレーザー光を照射する方
向と、レーザー光の照射により生じた散乱光を受光する
方向とが直交するように構成してもよい。 【0024】 【発明の効果】以上説明したように、本発明のラマン分
光分析と粒度分布測定を同時に行う分析装置は、レーザ
ー光源から試料に向けてレーザー光を照射し、生じたラ
マン散乱光のラマン・スペクトルを用いることで試料の
同定および定量分析を行うラマン分光分析器と、前記レ
ーザー光照射により生じた散乱光および透過光を用いて
粒度分布を測定する粒度分布測定器とよりなり、前記レ
ーザー光源をラマン分光分析と粒度分布測定に併用する
ことを特徴としたことにより、同一試料の同一部分に対
して、ラマン分光分析および粒度分布測定を同時に、正
確に、かつ迅速に行うことが可能となる。
Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an analyzer for simultaneously performing Raman spectroscopy and particle size distribution measurement. 2. Description of the Related Art A Raman spectrometer is one of devices for performing sample identification and quantitative analysis. In a conventional Raman spectrometer, a sample is analyzed by irradiating a sample with laser light (monochromatic light) and using a Raman spectrum of Raman scattered light generated. In order to measure the particle size distribution of a sample, a particle size distribution measuring device is used. In a conventional particle size distribution measuring device, a sample is irradiated with laser light (not limited to monochromatic light), and the particle size distribution of the sample is measured by using generated scattered light and transmitted light. When it is necessary to measure the particle size distribution of a certain sample together with the identification and quantitative analysis of the substance, the sample is measured with one device using both a Raman spectroscopic analyzer and a particle size distribution measuring device. After that, it was transported to the other device for measurement. [0005] However, in the above configuration, the measurement takes a long time because the sample is transported, and the properties of the sample change due to the elapse of this time and the transport of the sample. There was no quick and accurate analysis. The present invention has been made in consideration of the above-mentioned circumstances, and an object of the present invention is to simultaneously, accurately and rapidly perform Raman spectroscopic analysis and particle size distribution measurement on the same portion of the same sample. An object of the present invention is to provide an analyzer capable of simultaneously performing Raman spectroscopic analysis and particle size distribution measurement. In order to achieve the above object, an analyzer for simultaneously performing Raman spectroscopy and particle size distribution measurement according to the present invention irradiates a sample with laser light from a laser light source, Raman spectrometer for identifying and quantitatively analyzing samples by using Raman spectrum of generated Raman scattered light, and particle size distribution measurement for measuring particle size distribution using scattered light and transmitted light generated by the laser light irradiation The laser light source was used for Raman spectroscopy and particle size distribution measurement. With the above arrangement, Raman spectroscopic analysis and particle size distribution measurement are simultaneously performed on the same portion of the same sample.
An analyzer capable of performing Raman spectroscopic analysis and particle size distribution measurement that can be performed accurately and quickly can be provided. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The configuration of an analyzer for simultaneously performing Raman spectroscopy and particle size distribution measurement according to the present invention will be described with reference to the drawings. FIG. 1 is a diagram schematically showing a configuration of an analyzer D for simultaneously performing Raman spectroscopy and particle size distribution measurement according to one embodiment of the present invention. An analyzer D that simultaneously performs Raman spectroscopy and particle size distribution measurement is provided with a sample cell 1 in which a sample S is stored, a Raman spectrometer R provided on one side of the sample cell 1, and another side. And a particle size distribution measuring device P. The Raman spectrometer R irradiates the sample S with laser light from the laser light source 2 and performs identification and quantitative analysis of the sample S by using the Raman spectrum of the generated Raman scattered light. . The configuration is shown below. A laser light source 2 is provided upstream of the Raman spectrometer R. This laser light source 2
Laser light composed of monochromatic light (for example, 633 nm He-
Ne laser). The laser light emitted from the laser light source 2 passes through the lens 3 provided on the downstream side of the laser light source 2, the reflecting mirror 4, the beam splitter 5, and the lens 6, and reaches the sample cell 1. . The laser beam having passed through the lens 6 is applied to a sample S
Is applied to the focal position F of When the laser beam is applied to the focal position F, scattered light including Raman scattered light and Rayleigh scattered light is generated, and part of the generated scattered light passes through the lens 6 and the beam splitter 5 again. The light passes through the notch filter 7 and reaches the spectroscope 8. The notch filter 7 removes Rayleigh scattered light α having a large intensity as shown in a graph shown in an enlarged view of FIG. 1 in which frequency and scattered light intensity are plotted on the horizontal axis and the vertical axis, respectively. is there. Therefore, only the Raman scattered light reaches the spectroscope 8 via the notch filter 7. The spectroscope 8 has an optical sensor 9 (for example, a charge-coupled device), and a CPU 10 and a display unit 11 are connected downstream in this order. The display section 11 displays, for example, a graph in which the horizontal axis represents frequency and the vertical axis represents scattered light intensity, and the Raman spectrum of the obtained Raman scattered light can be visually recognized. . Further, by using the Raman spectrum, identification and quantitative analysis of the sample S can be performed, and concentration information of the sample S can be obtained. On the other hand, the particle size distribution measuring device P uses the scattered light and the transmitted light generated by the laser light applied to the sample S from the laser light source 2 of the Raman spectrometer R,
This is for measuring the particle size distribution of the sample S. The configuration is shown below. The laser light source 2 of the Raman spectrometer R
Is applied to the focal position F of the sample S, and transmitted light and scattered light are generated. Part of the transmitted light and the scattered light passes through a condenser lens 12 provided downstream of the sample cell 1 and passes through a photodetector 1 composed of a photodiode.
Reaches 3. Downstream of the photodetector 13 is a photodetector 13
, Which takes in the signal from the multiplexor, and the CPU 1 for receiving the signal from the multiplexer 14 and performing a calculation based on the scattered light intensity pattern to obtain a particle size distribution.
5. A display unit 16 for displaying the particle size distribution obtained by the CPU 15 is sequentially connected. The display section 16 displays, for example, a graph in which the horizontal axis indicates the particle size and the vertical axis indicates the frequency, so that the particle size distribution obtained by the measurement can be visually recognized. With the analyzer D having the above-described configuration for simultaneously performing Raman spectroscopy and particle size distribution measurement, simultaneous measurement of the same sample at the same position becomes possible, and analysis by a plurality of techniques can be realized quickly. In the analyzer D having the above structure for simultaneously performing Raman spectroscopic analysis and particle size distribution measurement, the Raman spectroscopic analyzer R and the particle size distribution measuring device P are appropriately connected to reflect each other's measurement results. If so, by reflecting the concentration information by Raman analysis in the particle size distribution calculation,
The reliability of particle size distribution measurement can be improved,
By reflecting the result of the particle size distribution measurement in the microanalysis of the Raman spectroscopic analysis, the reliability of the microanalysis using the Raman analysis can be improved. Of course, it is possible to easily determine the abnormality of both measurement systems. In the above configuration, the sample cell 1 is not limited to the one that stores the sample S, and may be, for example, a flow type that allows the sample S to flow inside, or a part of a pipe through which the sample S flows. Further, a window through which appropriate light is transmitted may be provided so as to have the same function as the sample cell on the flow side. With this configuration, the same analysis as described above can be performed on a sample in a flowing state using the analyzer D that simultaneously performs Raman spectroscopic analysis and particle size distribution measurement. In the above configuration, the direction of irradiating the focal position F of the sample S with the laser beam from the Raman spectrometer R and the direction of receiving the generated Raman scattered light, and the direction of the particle size distribution measuring device P May be provided so that the directions in which part of the transmitted light and the scattered light are received are all on a straight line, but the optical arrangement in the analyzer D for simultaneously performing Raman spectroscopic analysis and particle size distribution measurement of the present invention. Is not limited to this. For example, the direction in which the Raman spectrometer R irradiates laser light to the focal position F of the sample S and the direction in which scattered light generated by the irradiation of laser light is received are orthogonal to each other. May be configured. As described above, the analyzer for simultaneously performing Raman spectroscopy and particle size distribution measurement according to the present invention irradiates a laser beam from a laser light source toward a sample and generates Raman scattered light. A Raman spectrometer for performing sample identification and quantitative analysis by using a Raman spectrum, and a particle size distribution measuring device for measuring the particle size distribution using scattered light and transmitted light generated by the laser light irradiation, By using a laser light source for both Raman spectroscopy and particle size distribution measurement, it is possible to perform Raman spectroscopy and particle size distribution measurement simultaneously and accurately and quickly on the same part of the same sample. Becomes

【図面の簡単な説明】 【図1】本発明の一実施例に係るラマン分光分析と粒度
分布測定を同時に行う分析装置の構成を概略的に示す図
である。 【符号の説明】 2…レーザー光源、D…ラマン分光分析と粒度分布測定
を同時に行う分析装置、P…粒度分布測定器、R…ラマ
ン分光分析器、S…試料。
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a diagram schematically showing a configuration of an analyzer for simultaneously performing Raman spectroscopy and particle size distribution measurement according to one embodiment of the present invention. [Description of Signs] 2 ... Laser light source, D ... Analyzer that performs Raman spectroscopic analysis and particle size distribution measurement simultaneously, P ... Particle size distribution analyzer, R ... Raman spectroscopic analyzer, S ... Sample.

Claims (1)

(57)【特許請求の範囲】 【請求項1】 レーザー光源から試料に向けてレーザー
光を照射し、生じたラマン散乱光のラマン・スペクトル
を用いることで試料の同定および定量分析を行うラマン
分光分析器と、前記レーザー光照射により生じた散乱光
および透過光を用いて粒度分布を測定する粒度分布測定
器とよりなり、前記レーザー光源をラマン分光分析と粒
度分布測定に併用することを特徴とするラマン分光分析
と粒度分布測定を同時に行う分析装置。
(57) [Claims 1] Raman spectroscopy that irradiates a laser beam from a laser light source toward a sample and uses the Raman spectrum of the generated Raman scattered light to identify and quantitatively analyze the sample. An analyzer, comprising a particle size distribution measuring device that measures the particle size distribution using scattered light and transmitted light generated by the laser light irradiation, characterized in that the laser light source is used in combination with Raman spectroscopy and particle size distribution measurement. Analyzer that simultaneously performs Raman spectroscopy and particle size distribution measurement.
JP13804999A 1999-05-19 1999-05-19 An analyzer that simultaneously performs Raman spectroscopy and particle size distribution measurement Expired - Fee Related JP3422725B2 (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
JP13804999A JP3422725B2 (en) 1999-05-19 1999-05-19 An analyzer that simultaneously performs Raman spectroscopy and particle size distribution measurement

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Publication Number Publication Date
JP2000329682A JP2000329682A (en) 2000-11-30
JP3422725B2 true JP3422725B2 (en) 2003-06-30

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Country Status (1)

Country Link
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Publication number Priority date Publication date Assignee Title
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JP4266075B2 (en) * 2001-02-19 2009-05-20 株式会社堀場製作所 Particle size distribution measuring device
JP3858844B2 (en) * 2003-04-02 2006-12-20 日立協和エンジニアリング株式会社 Gas monitoring apparatus and gas monitoring method for underground fixation of carbon dioxide gas
US7333197B2 (en) * 2004-11-17 2008-02-19 Honeywell International Inc. Raman detection based flow cytometer
JP2012199359A (en) * 2011-03-22 2012-10-18 Sony Corp Laser irradiation device and microparticle measuring apparatus
EP2742337B1 (en) 2011-08-19 2016-05-04 Malvern Instruments Ltd Dual-mode characterization of particulates
CN105758770A (en) * 2015-11-03 2016-07-13 大族激光科技产业集团股份有限公司 Integrated substance component and granularity analyzing system and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103630523A (en) * 2012-08-21 2014-03-12 杭州希玛诺光电技术有限公司 Laser induction spectrum generating device used for water quality optical analyzer

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