JP3951577B2 - Method and apparatus for measuring turbidity and fine particles - Google Patents
Method and apparatus for measuring turbidity and fine particles Download PDFInfo
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- JP3951577B2 JP3951577B2 JP2000284611A JP2000284611A JP3951577B2 JP 3951577 B2 JP3951577 B2 JP 3951577B2 JP 2000284611 A JP2000284611 A JP 2000284611A JP 2000284611 A JP2000284611 A JP 2000284611A JP 3951577 B2 JP3951577 B2 JP 3951577B2
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- 239000010419 fine particle Substances 0.000 title claims description 71
- 238000000034 method Methods 0.000 title claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 52
- 239000002245 particle Substances 0.000 claims description 47
- 230000003287 optical effect Effects 0.000 claims description 25
- 230000000903 blocking effect Effects 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 241000195493 Cryptophyta Species 0.000 description 7
- 241000223935 Cryptosporidium Species 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は濁度および微粒子の測定方法とその装置に関する。
【０００２】
【従来の技術】
１９９６年のクリプトスポリジウム流出事故により、「クリプトスポリジウムによって水道原水が汚染されるおそれのある浄水場ではろ過池出口の濁度を０．１度以下に維持すること」という暫定対策指針が厚生省から発表され、濁度０．１度以下を安定に測定できるオンラインの濁度計が必要となった。そして、これまでに半導体レーザを光源に用い、微粒子が光ビームを通過する際に生じる回折縞をカウントし、カウント数を濁度に変換する特開平７−４９３０２号公報に記載のレーザ濁度計や、微粒子が光ビームを通過する際に、粒径に応じた波高値で観測される散乱光を粒径区分ごとにカウントし、カウントされた一つ一つの信号を微粒子の大きさに応じた濁度に変換する本発明者らが出願中の特開平１０−３１１７８４号公報に記載の微粒子カウント式高感度濁度計などが開発されている。また、前記事故以降の上水分野では、微粒子監視が普及し始めている。
【０００３】
微粒子カウンタの測定方式には、光ビームを試料水に照射し、光ビームの観測領域を微粒子が通過したときに生ずる散乱光パルス信号をカウントする散乱光方式と、光ビームの観測領域を微粒子が通過したときに生ずる、透過光量の減光パルス信号をカウントする光遮断方式とがある。光遮断方式の最小検出粒径は１〜２μｍであり、この粒径以上が光遮断方式の測定粒径となる。散乱光方式の最小検出粒径はパルス信号を検出する受光光学系の位置によって異なるが、側方散乱光方式で０．１μｍ以下、前方散乱光方式で０．１〜０．２μｍである。側方散乱方式では、前記クリプトスポリジウムなどの生物ように大きさがある程度揃い、屈折率が水に近い物質に対してほとんど感度を持たない場合があることが知られている。前方散乱光方式の場合は、前記生物のように光ビームの波長と比較して同程度以上に大きくなると、ほとんどが前方に向けて光ビームが散乱されるようになるので、側方散乱光方式と比較すると屈折率に対する影響は非常に小さいが、吸収成分を検出していない分だけ光遮断方式より粒径に対する感度が小さくなり、実際の大きさより小さい利粒子としてカウントされる場合がある。
【０００４】
上水分野では、クリプトスポリジウム相当径の４〜６μｍの粒子を監視することと、前記クリプトスポリジウムや浄水中にしばしば含まれる藻類は、校正に用いる標準粒子より屈折率が水に近いので、散乱光方式のパルス信号が小さくなるという理由から、主に光遮断方式が採用されている。
【０００５】
【発明が解決しようとする課題】
前記半導体レーザを用いた濁度計は、従来にない低濁度を安定して測定できるという利点を持つが、その反面、以下に述べる問題がある。その問題とは、濁度の測定値が手分析値（積分球方式）より小さくなる場合があることである。この原因は主に二つあり、その一つは前記半導体レーザを用いた濁度計は光ビームを絞っているため、ビーム幅以上の粒子が通過した場合、見かけの粒径が小さくカウントされてしまうことである。例えば、前記微粒子カウント式の場合、約１０μｍの粒子までは対応するが、それ以上の大きさの粒子は１０μｍ相当として濁度に変換されてしまうことがある。ほとんどの飲料水の中には１０μｍ以上の粒子が含まれていないため、通常は問題ないのであるが、藻類を多く含む原水を取水している浄水場などでは、凝集阻害などにより、ろ過水中に１０μｍ以上の粒子やフロックがしばしば検出され、濁度が手分析値より小さくなる場合がある。また、二つ目の原因は塩素と接触した藻類がろ過池から流出した場合、前記藻類は脱色によって散乱光が小さくなっているため、散乱光量の他に透過光量（吸収成分）を検出する積分球方式の濁度計より測定値が小さくなる場合があることである。
【０００７】
【課題を解決するための手段】
上記の問題を解決するため、請求項１から４の発明は濁度および微粒子の測定方法および測定装置（微粒子カウント式高感度濁度計および微粒子カウンタ）において、散乱光をカウントする散乱光方式の光学系と、微粒子が通過する際に減少する透過光量をパルスとしてカウントする光遮断方式を組み合わせることとする。
【０００９】
請求項１の発明は、集光された光ビームを試料水に向けて照射し、試料水中の微粒子によって散乱される光を光電変換素子で電気信号に変換する方法と、前記の光ビームとは異なる偏平光ビームを試料水に向けて照射し、試料水を透過する光を光電変換素子で電気信号に変換する方法とにより、予め定められた所定の粒径より小さい微粒子については、微粒子が前記集光された光ビームを通過する度に発生する散乱光パルス信号に基づいて粒径区分ごとに試料水中の微粒子の個数濃度を求め、また、前記所定の粒径より大きい微粒子については、微粒子が前記偏平光ビームを通過する度に発生する光遮断パルス信号に基づいて、粒径区分ごとに試料水中の微粒子の個数濃度を求め、さらに、前記微粒子の個数濃度に対して粒径区分ごとに個別の係数を乗じて試料水の濁度を求める濁度および微粒子の測定方法であることを特徴とする。
【００１０】
請求項２の発明は、集光された光ビームを試料水に向けて照射する光源と、前記集光された光ビームにより試料水中の微粒子によって散乱される光を光電変換素子で電気信号に変換する光電変換手段と、前記の光ビームとは異なる偏平光ビームを試料水に向けて照射する光源と、前記偏平光ビームにより試料水を透過する光を光電変換素子で電気信号に変換する光電変換手段とを有し、所定の粒径より小さい微粒子については、微粒子が前記集光された光ビームを通過する度に発生する散乱光パルス信号に基づいて、粒径区分ごとに試料水中の微粒子の個数濃度を求める計数手段と、また、前記所定の粒径より大きい微粒子については、微粒子が前記偏平光ビームを通過する度に発生する光遮断パルス信号に基づいて、粒径区分ごとに試料水中の微粒子の個数濃度を求める微粒子の計数手段と、さらに、前記微粒子の個数濃度に対して粒径区分ごとに個別の係数を乗じて試料水の濁度を求める手段とを備えた濁度および微粒子の測定装置であることを特徴とする。
【００１１】
請求項３の発明は、請求項２記載の濁度および微粒子の測定装置において、試料水が流れるフローセルに対して光源から光ビームを照射し、前記フローセルを介して、光源と対峙する位置で、かつ光ビームの光軸上に設置したビームストップにより光源からの直接の光ビームを遮断し、微粒子からの前方散乱光を検出する光学系と、光源から試料水が流れるフローセルに対して照射された偏平光の光量を検出する光学系を有することを特徴とする。
【００１２】
請求項４の発明は、請求項２記載の濁度および微粒子の測定装置において、試料水が流れるフローセルに対して光源から光ビームを照射し、試料水が流れる方向に垂直で、かつ前記光ビームの光軸に一定の角度の方向で、微粒子からの側方散乱光を検出する光学系と、試料水が流れるフローセルに対して光源から照射された偏平光の光量を検出する光遮断方式の光学系を有することを特徴とする。
【００１９】
【発明の実施の形態】
以下に本発明の実施形態について詳細に説明する。
〔実施例〕本発明の請求項１〜３に関する実施例として、微粒子による散乱光を検出する光学系に前方散乱光方式を採用した装置の光学系を図１に示す。図１の前方散乱光方式の光学系において、光源１から照射された光ビーム１Ａは、フローセル２の光ビーム照射領域を通過する試料水中の微粒子によって散乱される。試料水を通過する光源１からの直接光は、光源１から見てフローセル２の後ろ側に設置されたビームストップ３によって遮断され、ビームストップ３の外側を通過した前記微粒子による散乱光の一部は光ビームの光軸１Ｂと同一軸上に設置された集光レンズ系４によって集められ、迷光を遮るために設けたピンホール５を通過した後、前記光ビームの光軸１Ｂと同一軸上に設置された光電変換素子６によって電気信号に変換される。前記電気信号は図２のように光ビーム照射領域を微粒子が通過するたびに、微粒子の大きさに応じた波高値を持つ散乱光パルスとして検出される。
【００２０】
一方、図１のコネクタ１０によって、前方散乱光方式の光学系と接続された光遮断方式の光学系において、光源７から偏平に集光された光ビーム７Ａは、フローセル８の光ビーム照射領域を通過する試料水中の微粒子によって一部が遮蔽される。前記光ビームはその光軸７Ｂと同一軸上に設置された光電変換素子９によって電気信号に変換され、図３のように光ビーム照射領域を微粒子が通過するたびに、透過光が微粒子により減光した変化分としての微粒子の大きさに応じた波高値を持つ光遮断パルスとして検出される。
【００２１】
前記散乱光パルス信号と光遮断パルス信号は電子回路にて各々独立に増幅され、粒径に応じたしきい値とパルスの波高値を比較し、規定時間内に発生したパルスのカウント数が試料水中に含まれる微粒子個数濃度として出力される。ここで、例えば２μｍ未満の微粒子は前記散乱光パルス信号を基にカウントし、２μｍ以上の微粒子は光遮断パルス信号を基にカウントするようにしておけば、１μｍ以下の極微粒子から１００μｍ程度の微粒子までの幅広い粒径範囲で微粒子個数濃度を測定することが可能となる。また、特に塩素によって脱色された数μｍオーダーの藻類に対して、散乱光方式の微粒子カウンタより粒径感度の高い、光遮断方式によるパルスカウントが可能となる。
【００２２】
尚、本実施例では前方散乱光方式と光遮断方式の組合せを示したが、請求項４に関する側方散乱光方式と光遮断方式の組合せでも同じ効果が得られる。
【００３０】
【発明の効果】
本発明は微粒子および濁度の測定方法と、その装置にかかり、請求項１〜４の発明により一つの計測器で、サブミクロンから数百μｍの幅広い粒径レンジで微粒子の検出を可能とし、藻類や塩素により脱色された藻類、フロックに対する検出粒径の精度を向上させ、さらに微粒子カウント式濁度計に適用した場合は、積分球と同等の濁度測定値を得ることを可能とする。
【図面の簡単な説明】
【図１】実施例の装置で、微粒子による散乱光を検出する光学系として前方散乱光方式と光遮断方式とを組み合わせた光学系の構成と配置を示す図
【図２】実施例の装置における散乱光パルスの検出例を示す図
【図３】実施例の装置における光遮断パルスの検出例を示す図
【符号の説明】
１、７： 光源
１Ａ、７Ａ： 光ビーム
２、８： フローセル
３： ビームストップ
４： 集光レンズ系
１Ｂ、７Ｂ： 光ビームの光軸
５： ピンホール
６、９： 光電変換素子
１０： コネクタ[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method and apparatus for measuring turbidity and fine particles.
[0002]
[Prior art]
A provisional countermeasure guideline announced by the Ministry of Health, Labor and Welfare that the turbidity of raw water in a water treatment plant that may be contaminated by Cryptosporidium is maintained at 0.1 degrees or less at the basin outlet of the filtration basin due to a spill of Cryptosporidium in 1996 Therefore, an on-line turbidimeter that can stably measure turbidity of 0.1 degrees or less is required. A laser turbidimeter described in Japanese Patent Application Laid-Open No. 7-49302 that uses a semiconductor laser as a light source, counts diffraction fringes generated when fine particles pass through a light beam, and converts the count number to turbidity. Or, when the fine particles pass through the light beam, the scattered light observed at the crest value according to the particle size is counted for each particle size category, and each counted signal depends on the size of the fine particles. A fine particle count type high-sensitivity turbidimeter described in Japanese Patent Application Laid-Open No. 10-311784, which has been applied for by the present inventors to convert to turbidity, has been developed. In the field of water supply after the accident, particulate monitoring has begun to spread.
[0003]
The measurement method of the fine particle counter includes a scattered light method in which a sample beam is irradiated with a light beam and the scattered light pulse signal generated when the fine particle passes through the observation region of the light beam, and the observation region of the light beam is made up of fine particles. There is a light blocking method that counts a dimming pulse signal of a transmitted light amount that occurs when the light passes. The minimum detectable particle size of the light blocking method is 1 to 2 μm, and the particle size equal to or larger than this particle size is the measured particle size of the light blocking method. The minimum detection particle diameter of the scattered light method varies depending on the position of the light receiving optical system that detects the pulse signal, but is 0.1 μm or less in the side scattered light method and 0.1 to 0.2 μm in the forward scattered light method. It is known that the side-scattering method may have almost no sensitivity to a substance having a uniform size and a refractive index close to water, such as the living organism such as Cryptosporidium. In the case of the forward scattered light method, since the light beam is mostly scattered toward the front when it becomes larger than the wavelength of the light beam as in the case of the living thing, the side scattered light method Compared with, the influence on the refractive index is very small, but the sensitivity to the particle size is smaller than that of the light blocking method by the amount that the absorption component is not detected, and the particles may be counted as particles smaller than the actual size.
[0004]
In the water supply field, monitoring the Cryptosporidium equivalent diameter of 4 to 6 μm and the algae often contained in Cryptosporidium and purified water have a refractive index closer to water than the standard particles used for calibration, so scattered light The light blocking method is mainly adopted because the pulse signal of the method is small.
[0005]
[Problems to be solved by the invention]
The turbidity meter using the semiconductor laser, which has the advantage of low turbidity unprecedented can be stably measured, the other hand, there is a Ru problems described below. The their problem is that there are cases where the measured value of the turbidity is less than the manual analysis value (integrating sphere type). There are two main reasons for this. One of the causes is that the turbidimeter using the semiconductor laser narrows the light beam, so when particles larger than the beam width pass, the apparent particle size is counted small. It is to end. For example, in the case of the fine particle count method, particles up to about 10 μm are supported, but particles larger than that may be converted to turbidity as equivalent to 10 μm. Since most drinking water does not contain particles of 10 μm or more, there is usually no problem. However, in water purification plants that take in raw water containing a large amount of algae, it is not possible to add water to the filtered water due to coagulation inhibition. Particles and flocs of 10 μm or more are often detected, and the turbidity may be smaller than the manual analysis value. The second cause is that when algae in contact with chlorine flow out of the filter basin, the algae has a small amount of scattered light due to decolorization. The measured value may be smaller than that of a sphere type turbidimeter.
[0007]
[Means for Solving the Problems]
To solve the above problems, the invention of claims 1 to 4, in the measurement method and the measuring apparatus of turbidity and fine particle (particle count type sensitive turbidimeter and particle counter), of the scattered light method for counting the scattered light Assume that the optical system is combined with a light blocking method that counts the amount of transmitted light that decreases when fine particles pass as pulses.
[0009]
The invention of claim 1 is a method of irradiating a condensed light beam toward a sample water and converting light scattered by fine particles in the sample water into an electric signal by a photoelectric conversion element, and the light beam includes: By applying a different flat light beam toward the sample water and converting the light transmitted through the sample water into an electrical signal by the photoelectric conversion element, the fine particles are smaller than a predetermined particle diameter. The number concentration of fine particles in the sample water is determined for each particle size category based on the scattered light pulse signal generated each time the condensed light beam passes, and for fine particles larger than the predetermined particle size, The number concentration of the fine particles in the sample water is determined for each particle size category based on the light blocking pulse signal generated each time the flat light beam passes, and is further individually determined for each particle size category with respect to the number concentration of the fine particles. Wherein the multiplying coefficient is a measurement method of turbidity and fine seeking turbidity of sample water.
[0010]
According to a second aspect of the present invention, a light source that irradiates a sampled light beam toward the sample water, and light scattered by fine particles in the sample water by the collected light beam is converted into an electric signal by a photoelectric conversion element. Photoelectric conversion means, a light source for irradiating the sample water with a flat light beam different from the light beam, and photoelectric conversion for converting light transmitted through the sample water by the flat light beam into an electrical signal by a photoelectric conversion element A fine particle having a particle size smaller than a predetermined particle size, the fine particle in the sample water for each particle size category based on a scattered light pulse signal generated each time the fine particle passes through the condensed light beam. Counting means for determining the number concentration, and for fine particles larger than the predetermined particle size, the sample water for each particle size classification is based on a light blocking pulse signal generated each time the fine particles pass through the flat light beam. Fine particle counting means for determining the number concentration of fine particles, and means for determining the turbidity of sample water by multiplying the number concentration of the fine particles by an individual coefficient for each particle size category It is the measuring apparatus of this.
[0011]
According to a third aspect of the present invention, in the turbidity and particulate measurement device according to the second aspect, a light beam is irradiated from a light source to a flow cell through which sample water flows, and at a position facing the light source via the flow cell, In addition, an optical system that blocks the direct light beam from the light source by a beam stop installed on the optical axis of the light beam and detects the forward scattered light from the fine particles, and the flow cell through which the sample water flows are irradiated. It has an optical system for detecting the amount of flat light.
[0012]
According to a fourth aspect of the present invention, in the turbidity / fine particle measuring apparatus according to the second aspect, the light cell is irradiated with a light beam from a light source to the flow cell through which the sample water flows, and the light beam is perpendicular to the direction in which the sample water flows. An optical system that detects side scattered light from fine particles in a direction at a certain angle to the optical axis of the light, and a light blocking optical that detects the amount of flat light emitted from the light source to the flow cell through which the sample water flows It is characterized by having a system.
[0019]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail.
As an example of claims 1-3 EXAMPLES present invention, shown in FIG. 1 the optical system of the apparatus employing the forward scattered light method in the optical system for detecting the light scattered by the particles. In the forward scattered light type optical system of FIG. 1, the light beam 1 </ b> A irradiated from the light source 1 is scattered by fine particles in the sample water passing through the light beam irradiation region of the flow cell 2. Direct light from the light source 1 that passes through the sample water is blocked by the beam stop 3 installed behind the flow cell 2 when viewed from the light source 1, and part of the scattered light by the fine particles that has passed outside the beam stop 3. Are collected by a condensing lens system 4 installed on the same axis as the optical axis 1B of the light beam, pass through a pinhole 5 provided to block stray light, and then on the same axis as the optical axis 1B of the light beam. It is converted into an electric signal by the photoelectric conversion element 6 installed in. The electric signal is detected as a scattered light pulse having a peak value corresponding to the size of the fine particle every time the fine particle passes through the light beam irradiation region as shown in FIG.
[0020]
On the other hand, in the light blocking optical system connected to the forward scattered light optical system by the connector 10 in FIG. 1, the light beam 7 </ b> A collected flatly from the light source 7 passes through the light beam irradiation area of the flow cell 8. A part is shielded by the fine particles in the passing sample water. The light beam is converted into an electric signal by the photoelectric conversion element 9 installed on the same axis as the optical axis 7B, and the transmitted light is reduced by the fine particle every time the fine particle passes through the light beam irradiation region as shown in FIG. It is detected as a light blocking pulse having a peak value corresponding to the size of the fine particle as the amount of change that has been emitted.
[0021]
The scattered light pulse signal and the light blocking pulse signal are independently amplified by an electronic circuit, and the threshold value corresponding to the particle diameter is compared with the pulse peak value, and the number of pulses generated within a specified time is determined by the sample. Output as the number concentration of fine particles contained in water. Here, for example, if the fine particles of less than 2 μm are counted based on the scattered light pulse signal, and the fine particles of 2 μm or more are counted based on the light blocking pulse signal, the fine particles of 1 μm or less to about 100 μm It becomes possible to measure the fine particle number concentration in a wide range of particle sizes up to. In particular, for algae on the order of several μm decolorized by chlorine, it is possible to perform pulse counting by the light blocking method, which has a higher particle size sensitivity than the fine particle counter of the scattered light method.
[0022]
In this embodiment, the combination of the forward scattered light method and the light blocking method is shown, but the same effect can be obtained by the combination of the side scattered light method and the light blocking method related to claim 4 .
[0030]
【The invention's effect】
The present invention relates to a method for measuring fine particles and turbidity and an apparatus thereof. According to the inventions of claims 1 to 4, it is possible to detect fine particles with a single measuring instrument in a wide particle size range from submicron to several hundred μm. The accuracy of the detected particle size for algae and flocs decolorized by algae and chlorine is improved, and when applied to a fine particle count turbidimeter, it is possible to obtain a turbidity measurement value equivalent to that of an integrating sphere .
[Brief description of the drawings]
In Figure 1 apparatus of the embodiment, in FIG. 2 shows apparatus of the embodiment shown the arrangement and configuration of the optical system combining a forward scattered light method with light blocking scheme as an optical system for detecting light scattered by particles Figure [eXPLANATION oF sYMBOLS] showing an example of detection of the light blocking pulses in the apparatus of FIG. 1. FIG. 3 embodiment showing an example of detection of the scattered light pulse
1, 7: Light source 1A, 7A: Light beam 2, 8: Flow cell 3: Beam stop 4: Condensing lens system
1B , 7B: Optical axis of light beam 5: Pinhole 6, 9: Photoelectric conversion element 10: Connector
Claims (4)
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| JP2000284611A JP3951577B2 (en) | 2000-09-20 | 2000-09-20 | Method and apparatus for measuring turbidity and fine particles |
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| JP2007062224A Division JP4003809B2 (en) | 2007-03-12 | 2007-03-12 | Method and apparatus for measuring turbidity and fine particles |
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| CN111164389A (en) * | 2017-08-10 | 2020-05-15 | 联邦科学及工业研究组织 | Apparatus and method for monitoring material flow parameters along a channel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111164389A (en) * | 2017-08-10 | 2020-05-15 | 联邦科学及工业研究组织 | Apparatus and method for monitoring material flow parameters along a channel |
| CN111164389B (en) * | 2017-08-10 | 2022-09-02 | 联邦科学及工业研究组织 | Apparatus and method for monitoring material flow parameters along a channel |
| US11536597B2 (en) | 2017-08-10 | 2022-12-27 | Commonwealth Scientific And Industrial Research Organisation | Device and method for monitoring material flow parameters along a passage |
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