JP3499009B2 - Particle size distribution analyzer - Google Patents
Particle size distribution analyzerInfo
- Publication number
- JP3499009B2 JP3499009B2 JP20987694A JP20987694A JP3499009B2 JP 3499009 B2 JP3499009 B2 JP 3499009B2 JP 20987694 A JP20987694 A JP 20987694A JP 20987694 A JP20987694 A JP 20987694A JP 3499009 B2 JP3499009 B2 JP 3499009B2
- Authority
- JP
- Japan
- Prior art keywords
- particles
- signal
- solution
- detected
- particle size
- 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
Links
- 239000002245 particle Substances 0.000 title claims description 158
- 239000007788 liquid Substances 0.000 claims description 99
- 238000001514 detection method Methods 0.000 claims description 72
- 239000000523 sample Substances 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 24
- 230000008859 change Effects 0.000 claims description 23
- 239000012488 sample solution Substances 0.000 claims description 17
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 4
- 239000002612 dispersion medium Substances 0.000 claims description 4
- 239000012510 hollow fiber Substances 0.000 claims description 4
- 238000003921 particle size analysis Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 102000003743 Relaxin Human genes 0.000 claims description 3
- 108090000103 Relaxin Proteins 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- PNVNVHUZROJLTJ-UHFFFAOYSA-N venlafaxine Chemical compound C1=CC(OC)=CC=C1C(CN(C)C)C1(O)CCCCC1 PNVNVHUZROJLTJ-UHFFFAOYSA-N 0.000 claims description 2
- 229960004688 venlafaxine Drugs 0.000 claims description 2
- 102000010970 Connexin Human genes 0.000 claims 1
- 108050001175 Connexin Proteins 0.000 claims 1
- 230000032683 aging Effects 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 239000000284 extract Substances 0.000 claims 1
- 238000000691 measurement method Methods 0.000 claims 1
- 239000002609 medium Substances 0.000 claims 1
- 239000000725 suspension Substances 0.000 description 63
- 239000000243 solution Substances 0.000 description 42
- 239000011148 porous material Substances 0.000 description 26
- 210000004027 cell Anatomy 0.000 description 16
- 230000003321 amplification Effects 0.000 description 9
- 238000003199 nucleic acid amplification method Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- 238000000605 extraction Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000000601 blood cell Anatomy 0.000 description 2
- 210000001124 body fluid Anatomy 0.000 description 2
- 239000010839 body fluid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 210000002751 lymph Anatomy 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 210000002700 urine Anatomy 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 210000003743 erythrocyte Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 210000000265 leukocyte Anatomy 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000007415 particle size distribution analysis Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、各種の流体や微粒子
の粒度分析を測定する装置に関し、さらに詳しくは、測
定する粒子懸濁液を別の液体と共に細流化して流すシー
スフロー方式を用い、粒度分布を電気的検知帯法で測定
する粒度分布測定装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for measuring the particle size analysis of various fluids and fine particles, and more specifically, it uses a sheath flow system in which a particle suspension to be measured is made to trickle with another liquid, The present invention relates to a particle size distribution measuring device for measuring particle size distribution by an electrical detection zone method.
【０００２】[0002]
【従来の技術】ファインセラミックス粒子、顔料、ある
いは化粧品用パウダー等の粉体の品質を管理する上で、
粒子の粒径を測定、管理することが非常に重要である。
その測定装置として、古くから液相沈降法、電気的検知
帯法による測定装置があり、最近ではレーザ回折散乱法
による測定装置が広く利用されている。2. Description of the Related Art In controlling the quality of fine ceramic particles, pigments or powders for cosmetics,
It is very important to measure and control the particle size of particles.
As a measuring device therefor, there has been a measuring device by a liquid phase sedimentation method or an electric detection zone method since ancient times, and a measuring device by a laser diffraction scattering method has been widely used recently.
【０００３】電気的検知帯法による装置は、電解液に浮
遊させた粒子が小さな穴を通過する時の電気抵抗の変化
量を検出するものであり、１個１個の粒子の体積相当径
が形状にほとんど影響されずに測定できるという利点を
有している。ただし従来の電気的検知帯法による装置で
は、粒子が細孔部（アパーチャ）の端を通過することが
多くあり、このような粒子に対しては正確な粒子体積を
求めることはできない。An apparatus based on the electrical detection zone method detects the amount of change in electrical resistance when particles suspended in an electrolytic solution pass through a small hole, and the volume equivalent diameter of each particle is It has an advantage that it can be measured without being affected by the shape. However, in the conventional apparatus using the electrical detection zone method, particles often pass through the ends of the pores (apertures), and an accurate particle volume cannot be obtained for such particles.
【０００４】この問題を解決する方法として、粒子懸濁
液の流れを別の液体（シース液）で取り囲むようにする
ことによって、懸濁液流を細く絞った状態で細孔部に導
入する方式、すなわちシースフロー方式が知られてい
る。この方式では、粒子は細孔のほぼ中心を通過するの
で、より正確な粒度分布が測定できる。たとえば、特開
昭５０−４６１７９号公報には、電気伝導度を監視しそ
の変化に基づき検出信号の大きさを補正する粒子分析装
置が記載されている。As a method for solving this problem, a method in which a suspension liquid is surrounded by another liquid (sheath liquid) so that the suspension liquid is introduced into the fine pores in a state of being narrowed down That is, the sheath flow method is known. In this method, the particles pass through almost the center of the pores, so that a more accurate particle size distribution can be measured. For example, Japanese Patent Application Laid-Open No. 50-46179 discloses a particle analyzer which monitors electric conductivity and corrects the magnitude of a detection signal based on the change.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、このシ
ースフロー方式による粒度分布測定装置では、さまざま
な種別や大きさの粉体を測定するために、細孔径の異な
る細孔部を予め用意しておく必要があるほか、次のよう
な問題がある。However, in this sheath flow type particle size distribution measuring apparatus, in order to measure powders of various types and sizes, pore portions having different pore diameters are prepared in advance. In addition to the above, there are the following problems.
【０００６】一般的に粒子が小さくなるほど粒子どうし
で凝集しやすくなり正しく粒度分析を測定するのが難し
くなる。この粒子どうしの凝集を抑えるための方法とし
て、粒子懸濁液に分散剤を添加する方法が一般的である
が、粉体の種類によって最適な分散剤は異なる。Generally, the smaller the particles are, the more likely they are to agglomerate with each other, which makes it difficult to measure particle size analysis correctly. As a method for suppressing the aggregation of the particles, a method of adding a dispersant to the particle suspension is generally used, but the optimum dispersant varies depending on the type of powder.
【０００７】このような、粒子どうしの凝集を抑えるた
めの分散剤の添加、あるいは粒子自身からの析出物質等
による影響により、粒子懸濁液の電気伝導度がシース液
の電気伝導度と一致しないことがある。すなわちシース
フロー電気インピーダンス方式による粒子検出を行う場
合に、試料液流の特性とシース液の特性たとえば電気伝
導度が異なると、信号のゆらぎやリニアリティがなくな
るなどの問題が生じる。The electrical conductivity of the particle suspension does not match the electrical conductivity of the sheath liquid due to the addition of the dispersant for suppressing the agglomeration of the particles or the influence of the precipitation substance from the particles themselves. Sometimes. That is, when particles are detected by the sheath flow electrical impedance method, if the characteristics of the sample liquid flow and the characteristics of the sheath liquid, such as electrical conductivity, are different, problems such as signal fluctuations and linearity disappear.
【０００８】例えば、試料を血液とし血球の検出を行う
場合には、通常元の試料は所定の試薬により数百倍に希
釈する。また、試料によっては、希釈せずに試料をその
まま測定したい場合もあり、測定対象を広げて行くと試
料液の特性とシース液の特性が異なる場合に遭遇する。
このため、希釈用試薬の電気伝導度とシース液の電気伝
導度とが一致しない状況が起こりえるので、上記のよう
な問題が発生し正確な粒度分布や粒子の体積が測定でき
ないおそれがある。具体的には、懸濁液とシース液の流
量比が安定していないと、細孔部の電気抵抗値がふらつ
き、検出信号にゆらぎが生じる。For example, when blood cells are used as a sample for detection of blood cells, the original sample is usually diluted several hundred times with a predetermined reagent. In addition, depending on the sample, there is a case where it is desired to measure the sample as it is without dilution, and when the measurement target is expanded, the case where the characteristics of the sample liquid and the characteristics of the sheath liquid differ is encountered.
For this reason, the electric conductivity of the diluting reagent and the electric conductivity of the sheath liquid may not coincide with each other, so that the above-mentioned problems may occur and accurate particle size distribution and particle volume may not be measured. Specifically, if the flow rate ratio of the suspension liquid and the sheath liquid is not stable, the electric resistance value of the pore portion fluctuates, and the detection signal fluctuates.
【０００９】また、細孔部における懸濁液流の太さより
大きな粒子が通過する場合、電気の流れに対する粒子の
妨害は、懸濁液流とシース液流の両方にまたがり、双方
の液の電気伝導度が異なると、電気抵抗の変化量が粒子
の大きさに比例しなくなる。すなわちリニアリティがな
くなる。Further, when particles larger than the thickness of the suspension flow in the pores pass through, the interference of the particles with respect to the flow of electricity extends over both the suspension flow and the sheath liquid flow, and the electric flow of both liquids is disturbed. When the conductivity is different, the amount of change in electric resistance is not proportional to the size of the particles. That is, there is no linearity.
【００１０】このようなリニアリティ等の問題に対する
対策方法として、粒子懸濁液の流量に対してシース液の
流量の比率を極力大きくすること、すなわちシース液流
の断面積に比べてサンプル流の断面積を非常に小さくす
ることによって、懸濁液の電気伝導度との差による影響
を極力小さくする方法が提案されている。例えば、シー
ス液流量を懸濁液流量の2500倍にすると、細孔部での懸
濁液流の径は、細孔径の約２％（＝１／５０）になる。
従って、細孔部の約５％以上の径の粒子については、懸
濁液の電気伝導度による影響はほとんど無視することが
でき、粒子の大きさに比例した電気抵抗変化が得られ
る。As a countermeasure against such a problem as linearity, the ratio of the flow rate of the sheath liquid to the flow rate of the particle suspension should be maximized, that is, the sample flow should be cut off as compared with the cross-sectional area of the sheath liquid flow. A method has been proposed in which the influence of the difference from the electrical conductivity of the suspension is minimized by making the area very small. For example, if the flow rate of the sheath liquid is 2500 times the flow rate of the suspension, the diameter of the suspension flow in the pores is about 2% (= 1/50) of the pore diameter.
Therefore, for particles having a diameter of about 5% or more of the pores, the influence of the electrical conductivity of the suspension can be almost ignored, and an electric resistance change proportional to the size of the particles can be obtained.
【００１１】しかしながら、この対策方法では、懸濁液
流の径に近い小さな粒子については、懸濁液とシース液
の電気伝導度の差による影響を受け、正しく粒度を測定
することができない。また、懸濁液流の径が細いので、
単位時間当たりの試料分析量が少なく、短時間で再現性
のある粒度測定ができない。細孔部を通過する液流の速
度を上げることによって試料分析量をかせぐことができ
るが、シース液消費量が増大するだけでなく、電気抵抗
検出信号の周波数帯域が高くなり、Ｓ／Ｎが悪化すると
いう問題点がある。However, with this countermeasure, small particles having a diameter close to the diameter of the suspension flow cannot be accurately measured due to the influence of the difference in electric conductivity between the suspension and the sheath liquid. Also, since the diameter of the suspension flow is small,
The amount of sample analyzed per unit time is small and reproducible particle size measurement cannot be performed in a short time. Although the sample analysis amount can be gained by increasing the velocity of the liquid flow passing through the fine pores, not only the sheath liquid consumption amount increases but also the frequency band of the electric resistance detection signal increases and the S / N ratio increases. There is a problem that it gets worse.
【００１２】この発明は、以上のような事情を考慮して
なされたものであり、測定する粒子懸濁液から抽出した
溶液をシース液として利用することによって、粒子懸濁
液とシース液の電気伝導度が異なる場合に生じる問題点
を解決し、正しく粒度分布を測定することができる粒度
分布測定装置を提供することを目的とする。また、粒子
懸濁液の電気伝導度に相当する電気信号を検出すること
によって、測定する粒子の大きさが正しく検出できるよ
うな補正を行う粒度分布測定装置を提供することを目的
とする。The present invention has been made in consideration of the above circumstances, and by using a solution extracted from a particle suspension to be measured as a sheath liquid, the electrical conductivity of the particle suspension and the sheath liquid can be improved. An object of the present invention is to provide a particle size distribution measuring device capable of solving the problems that occur when the conductivity is different and accurately measuring the particle size distribution. Another object of the present invention is to provide a particle size distribution measuring device that corrects the size of particles to be measured by detecting an electric signal corresponding to the electric conductivity of the particle suspension.
【００１３】[0013]
【課題を解決するための手段】この発明は、シースフロ
ー方式の電気的検知帯法による粒度分布測定装置におい
て、被検出粒子と導電性分散媒と分散剤とを含む試料液
を収容する容器と、前記容器から供給された被検出粒子
を検出するための検出孔部と、被検出粒子を含む試料液
を検出孔部に導く前室と、検出孔部から流出した前記試
料液を排出する後室とを備える測定手段と、前記試料液
から被検出粒子を除き溶液成分のみを抽出する溶液抽出
手段と、前記溶液抽出手段によって抽出される溶液成分
をシース液として前記測定手段に供給するシース液供給
手段と、被検出粒子が前記検出孔部を通過する際の電気
抵抗の変化を電気信号として検知する信号検知手段とを
備えることを特徴とする粒度分布測定装置を提供するも
のである。The present invention relates to a particle size distribution measuring apparatus using a sheath flow type electric detection zone method , and a sample liquid containing particles to be detected, a conductive dispersion medium and a dispersant.
A container for containing, a detection hole portion for detecting the particles to be detected supplied from the container , a front chamber for guiding a sample solution containing the particles to be detected to the detection hole portion, and the sample flowing out from the detection hole portion The measuring means having a rear chamber for discharging the liquid, the solution extracting means for extracting only the solution component from the sample liquid by removing the particles to be detected, and the measuring means using the solution component extracted by the solution extracting means as the sheath liquid. (EN) A particle size distribution measuring device comprising: a sheath liquid supplying means for supplying to the above; and a signal detecting means for detecting a change in electric resistance when a particle to be detected passes through the detection hole portion as an electric signal. It is a thing.
【００１４】また、前記シース液供給手段が、前記測定
手段の前室及び後室に前記シース液を供給するようにす
ることが好ましい。さらに、前記溶液抽出手段が、中空
糸フィルタを備えることが好ましい。Further, it is preferable that the sheath liquid supply means supplies the sheath liquid to the front chamber and the rear chamber of the measuring means. Furthermore, it is preferable that the solution extracting means includes a hollow fiber filter.
【００１５】 また、前記信号検知手段によって検知さ
れた電気信号のＤＣ成分を抽出し、このＤＣ成分信号を
利用して前記電気信号のレベルを補正する補正手段を備
え、前記補正手段が被検出粒子の粒度分布に対応する測
定信号を生成するようにすることが好ましい。Further, to extract the DC component of the electrical signal detected by the signal detecting means, a correction means for correcting a level of the electrical signal by using the DC component signal, before Symbol correction means to be detected It is preferable to generate a measurement signal corresponding to the particle size distribution of the particles.
【００１６】 ここで前記信号検知手段が、前記測定手
段の前室及び後室に配置される一対の電極を備え、この
電極間の電圧に対応する電気信号を検知し、前記補正手
段が前記電気信号のＤＣ成分信号によって電気信号の増
幅率を調整することが好ましい。また、この発明は、被
検出粒子と導電性分散媒と分散剤とを攪拌することによ
って試料液を調製する工程と、前記試料液を吸引する工
程と、前記試料液から被検出粒子を除き溶液成分のみを
抽出してシース液を調製する工程と、被検出粒子を検出
するための検出孔部と、前記試料液を検出孔部に導く前
室と、検出孔部から流出した前記試料液を排出する後室
とを備える測定手段に、前記試料液及びシース液を導く
工程と、被検出粒子が前記検出孔部を通過する際の電気
抵抗の変化を電気信号として検知する工程と、電気信号
に基づいて粒度分布を得る工程と、からなる粒度分布測
定方法を提供するものである。 [0016] A wherein said signal detecting means, wherein a pair of electrodes disposed in the front chamber and the rear chamber of the measuring means, detects that electrostatic No. venlafaxine corresponding to the voltage between the electrodes, wherein the correction means it is preferable to adjust the amplification factor of No. conductive relaxin by DC component signal of the photoelectric No. relaxin. In addition, the present invention is
By stirring the detection particles, the conductive dispersion medium, and the dispersant.
To prepare a sample solution and to suck the sample solution
And remove the particles to be detected from the sample solution and leave only the solution component.
Extraction to prepare sheath liquid and detection of particles to be detected
Before introducing the sample solution to the detection hole
Chamber and rear chamber for discharging the sample liquid flowing out from the detection hole
The sample liquid and the sheath liquid are guided to the measuring means including
Process and electricity when particles to be detected pass through the detection hole
The process of detecting the change in resistance as an electrical signal, and the electrical signal
The process of obtaining a particle size distribution based on
It provides a fixed method.
【００１７】また前記測定装置の検出孔部が、前室及び
後室とに分離できる構造を有することが好ましい。ま
た、検出孔部は、被検出粒子を検出するための細孔を有
することが好ましい。Further, it is preferable that the detection hole portion of the measuring device has a structure capable of being separated into a front chamber and a rear chamber. Further, it is preferable that the detection hole portion has a fine hole for detecting the particles to be detected.
【００１８】ここで、測定対象となる粒子としては、微
粒子、微生物、及び生体細胞などが上げられる。これら
の粒子を含有する試料液としては、例えば、血液、リン
パ液、尿などの体液が用いられ、この場合は、赤血球や
白血球などの生体粒子細胞が測定対象となる。Here, the particles to be measured include fine particles, microorganisms, and living cells. As the sample liquid containing these particles, for example, a body fluid such as blood, lymph, or urine is used, and in this case, biological particle cells such as red blood cells and white blood cells are to be measured.
【００１９】測定手段の例としては、いわゆるフローサ
イトメータがあるが、これは測定対象の粒子を含む試料
液と、この試料液を絞り込むためにこの液の回りに流す
シース液とからなる懸濁液を細流化して流し、粒子の数
や大きさを測定するものである。溶液抽出手段は、試料
液を中空糸フィルタなどを用いてろ過することで試料液
中の溶液成分を捕捉するものであり、試料液を流入する
前室部と、その試料液が流出する後室部と、前室部及び
後室部を区分するように設けられその試料液中の溶液成
分を捕捉するフィルタ部とからなる。ここで、前室部へ
の試料の流入、後室からの溶液成分の流出は、たとえば
シリンジの操作により行われる。As an example of the measuring means, there is a so-called flow cytometer, which is a suspension consisting of a sample liquid containing particles to be measured and a sheath liquid flowing around this liquid to narrow down the sample liquid. The liquid is made into a fine stream and then poured to measure the number and size of particles. The solution extraction means captures the solution components in the sample solution by filtering the sample solution using a hollow fiber filter, etc., and the front chamber into which the sample solution flows and the rear chamber from which the sample solution flows out. And a filter part which is provided so as to divide the front chamber part and the rear chamber part so as to capture the solution component in the sample liquid. Here, the inflow of the sample into the front chamber and the outflow of the solution component from the rear chamber are performed, for example, by operating a syringe.
【００２０】シース液供給手段は、溶液抽出手段によっ
て抽出された溶液をシース液として測定手段に供給する
ものであり、抽出された溶液を蓄えるチャンバと、チャ
ンバに蓄えられた溶液を測定手段に送るための圧力を加
える空圧源とを備えることが好ましい。The sheath liquid supplying means supplies the solution extracted by the solution extracting means to the measuring means as a sheath liquid, and sends a chamber for storing the extracted solution and the solution stored in the chamber to the measuring means. It is preferable to provide an air pressure source for applying a pressure.
【００２１】信号検知手段は、前記したような１対の電
極を備えることが好ましいが、さらにこの一対の電極間
に一定の電流を流すことができるように制御を行う定電
流源を備えることが好ましい。The signal detecting means preferably comprises a pair of electrodes as described above, but may further comprise a constant current source for controlling so that a constant current can flow between the pair of electrodes. preferable.
【００２２】補正手段は、入力される電気信号のＤＣ成
分を抽出するフィルタ回路と電圧制御増幅器を備え、入
力される電気信号をアナログ信号レベルで補正してもよ
い。ここで、フィルタ回路は、ＤＣ成分を抽出するため
の低域通過フィルタと、このフィルタで通過した信号の
電圧レベルを保持するサンプルホルダーとから構成され
ることが好ましい。また、電圧制御増幅器は、ＤＣ成分
によって決められる所定の基準の増幅率に従って電気信
号を増幅することによって補正する。The correction means may include a filter circuit for extracting the DC component of the input electric signal and a voltage control amplifier, and correct the input electric signal at the analog signal level. Here, the filter circuit is preferably composed of a low-pass filter for extracting the DC component and a sample holder for holding the voltage level of the signal passed by this filter. Further, the voltage control amplifier corrects the electric signal by amplifying the electric signal according to a predetermined reference amplification factor determined by the DC component.
【００２３】ここでの補正の基準となる電気信号のＤＣ
成分は、測定する粒子が細孔を通過していない場合の電
気信号を意味し、このレベルを基準として、補正量が決
められる。すなわち、測定された電気信号のＤＣ成分の
レベル信号と、基準となるＤＣ成分のレベル信号とか
ら、電圧制御増幅器の増幅率が決められ、測定された電
気信号のレベルがこの増幅率によって補正される。特
に、一対の電極間の電圧を測定する場合には、上記の入
力される電気信号は電気抵抗検出信号を意味する。ま
た、補正手段として、マイクロコンピュータを用い、入
力される電気信号をＡ／Ｄ変換した後、所定の補正を行
ってもよい。DC of the electric signal which is the reference of the correction here
The component means an electric signal when the particles to be measured do not pass through the pores, and the correction amount is determined based on this level. That is, the amplification factor of the voltage controlled amplifier is determined from the measured DC component level signal of the electric signal and the reference DC component level signal, and the measured electric signal level is corrected by this amplification factor. It In particular, when measuring the voltage between a pair of electrodes, the input electric signal means an electric resistance detection signal. Further, a microcomputer may be used as the correction means, and the predetermined correction may be performed after A / D conversion of the input electric signal.
【００２４】[0024]
【作用】この発明によれば、被検出粒子を含む試料液か
ら溶液成分のみを抽出して、これをシース液として測定
手段に供給しているので、試料液とシース液の電気伝導
度が異なることのないようにでき正しく粒度分布を測定
することができる。また、測定手段の後室にシース液を
供給するので、検出孔部を通過した粒子の舞い戻りを防
ぐことができる。According to the present invention, since only the solution component is extracted from the sample liquid containing the particles to be detected and supplied as the sheath liquid to the measuring means, the sample liquid and the sheath liquid have different electric conductivities. It is possible to measure the particle size distribution correctly. Further, since the sheath liquid is supplied to the rear chamber of the measuring means, it is possible to prevent the particles that have passed through the detection hole from returning.
【００２５】また、被検出粒子が検出孔部を通過する際
に生じる電気信号のＤＣ成分を検出しているので、懸濁
液の電気伝導度が異なる場合でも、測定する粒子の大き
さが正しく検出できるように電気信号のレベルを補正で
きる。また、前記測定装置の検出孔部が前室及び後室と
分離できる構造を持つため、検出孔部を孔径の異なる細
孔を持つ他の検出孔部と交換することができ、種々の大
きさを持つ粒子の粒度分布を測定することが可能であ
る。Further, since the DC component of the electric signal generated when the particles to be detected pass through the detection hole portion is detected, the size of the particles to be measured is correct even if the electric conductivity of the suspension is different. The level of the electrical signal can be corrected so that it can be detected. Further, since the detection hole portion of the measuring device has a structure that can be separated from the front chamber and the rear chamber, the detection hole portion can be replaced with another detection hole portion having pores with different hole diameters, and various sizes can be obtained. It is possible to measure the particle size distribution of particles with.
【００２６】[0026]
【実施例】以下、図面に示す実施例に基づいてこの発明
を詳述する。なお、これによってこの発明が限定される
ものではない。図１にこの発明の粒度分布装置における
実施例の構成ブロック図を示す。図１において、１は測
定する粒子が含まれる試料液すなわち粒子懸濁液であ
り、２は吸引ピペットで、３はフィルタユニットで、４
はフィルタユニット３に導かれた粒子懸濁液のうち溶液
成分を取り出す溶液抽出用シリンジである。ここで、フ
ィルタユニット３は、ポリエチレンなどの材質を使用い
た親水性の中空糸フィルタを用いるのが好ましい。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail with reference to the embodiments shown in the drawings. The present invention is not limited to this. FIG. 1 is a block diagram showing the configuration of an embodiment of the particle size distribution device of the present invention. In FIG. 1, 1 is a sample liquid containing particles to be measured, that is, a particle suspension, 2 is a suction pipette, 3 is a filter unit, and 4 is a filter unit.
Is a solution extraction syringe for taking out a solution component from the particle suspension guided to the filter unit 3. Here, as the filter unit 3, it is preferable to use a hydrophilic hollow fiber filter made of a material such as polyethylene.
【００２７】図３にフィルタユニット３の実施例を示
す。ここで、フィルタユニット３は、粒子懸濁液が流入
する前室３ａと、粒子懸濁液の溶液成分が流出する後室
３ｂと、前室と後室を区分するように設けられたフィル
タ材料３ｃとから構成される。フィルタ材料３ｃは溶液
成分は通すが、粒子を通過させない孔を有している。溶
液抽出用シリンジ４が吸引動作をすると、溶液成分のみ
が前室３ａからフィルタ材料３ｃを通過して後室３ｂに
抽出される。このとき測定する粒子のみが前室３ａ内に
残留する。FIG. 3 shows an embodiment of the filter unit 3. Here, the filter unit 3 is provided with a front chamber 3a into which the particle suspension flows in, a rear chamber 3b into which a solution component of the particle suspension flows out, and a filter material provided so as to separate the front chamber and the rear chamber. 3c. The filter material 3c has pores that allow the solution components to pass through but do not allow particles to pass through. When the solution extracting syringe 4 performs the suction operation, only the solution component is extracted from the front chamber 3a through the filter material 3c to the rear chamber 3b. Only the particles measured at this time remain in the front chamber 3a.
【００２８】後室３ｂに抽出された溶液成分は、後述す
るシース液チャンバ６に蓄えられて、シース液として利
用される。すなわち、測定する粒子懸濁液とこのように
して得られたシース液の溶液成分とは同一であるため、
電気的検知帯法による測定に寄与する粒子懸濁液とシー
ス液との電気伝導度を一致させることができ、正確な粒
度分析測定が可能となる。The solution component extracted in the rear chamber 3b is stored in a sheath liquid chamber 6 described later and used as a sheath liquid. That is, since the particle suspension to be measured and the solution component of the sheath liquid thus obtained are the same,
The electrical conductivity of the particle suspension that contributes to the measurement by the electrical detection zone method and the electric conductivity of the sheath liquid can be matched, and accurate particle size analysis measurement can be performed.
【００２９】また、空圧源５は、シース液チャンバ６に
シース液送出圧１５をかけ、廃液チャンバ８に懸濁液吸
収圧１６をかけるためのものである。シース液チャンバ
６は、溶液成分ライン１０から送られる溶液を貯蔵する
ための容器であり、ここからシースフローセル７にシー
ス液が供給される。シースフローセル７は、粒子懸濁液
をシース液とを細流化して流し、粒子の分類測定を行う
装置である。The air pressure source 5 is for applying a sheath liquid delivery pressure 15 to the sheath liquid chamber 6 and a suspension absorption pressure 16 to the waste liquid chamber 8. The sheath liquid chamber 6 is a container for storing the solution sent from the solution component line 10, and the sheath liquid is supplied to the sheath flow cell 7 from here. The sheath flow cell 7 is a device for classifying and measuring particles by flowing a particle suspension into a sheath liquid and making it flow into a narrow stream.
【００３０】図２に、このシースフローセル７の構成図
の例を示す。同図において、サンプルノズル２１を通し
て、粒子懸濁液３１が流入させられ、その横の入口か
ら、フロントシース液３２が流入させられる。２２は検
出孔部であり、粒子懸濁液３１とフロントシース液３２
を細流化して流すものであり、その中央部に細孔２６を
有する。FIG. 2 shows an example of a configuration diagram of the sheath flow cell 7. In the figure, the particle suspension 31 is made to flow in through the sample nozzle 21, and the front sheath liquid 32 is made to flow in from the inlet on the side thereof. Reference numeral 22 denotes a detection hole portion, which is a particle suspension 31 and a front sheath liquid 32.
Is made into a narrow stream, and has a pore 26 in the center thereof.
【００３１】この、検出孔部２２は種々の大きさの粒子
を測定できるように、脱着式であることが好ましく、孔
径の異なる検出孔部２２に容易に交換できるような構造
となっていることが好ましい。たとえば、何種類かの径
の細孔２６を有する円板状のディスク又はバーを回転あ
るいはスライドさせて容易に径を選択できるものがよ
い。The detection hole portion 22 is preferably of a detachable type so that particles of various sizes can be measured, and has a structure that can be easily replaced with the detection hole portion 22 having a different hole diameter. Is preferred. For example, it is preferable that the diameter can be easily selected by rotating or sliding a disc-shaped disk or bar having pores 26 of several kinds of diameters.
【００３２】３３は、フロントシース液３２と同じ溶液
成分のバックシース液であり、検出孔部２２を通過した
粒子の舞い戻りを防ぐためのものであり、粒子と共に回
収管２４を通って廃液チャンバ８へ流出される。Reference numeral 33 is a back sheath liquid having the same solution component as the front sheath liquid 32, which is for preventing the particles that have passed through the detection hole portion 22 from returning to the waste liquid chamber 8 through the recovery pipe 24 together with the particles. Is leaked to.
【００３３】また、シースフローセル７の内部でフロン
トシース液３２が流入する部分とバックシース液３３が
流入する部分に電極２３が配置させられる。この電極２
３はシースフローセル７の中を流れる液体の電気抵抗値
を測定するためのものであり、常時定電流源２５によっ
て電極間に一定電流を流しておき、粒子が検出孔部２２
を通過するときに変化する電極間電圧が測定される。こ
の電極間電圧は、電気抵抗検出信号１７として取り出さ
れ、後述する信号処理部によって処理される。Further, the electrodes 23 are arranged inside the sheath flow cell 7 at a portion into which the front sheath liquid 32 flows and a portion into which the back sheath liquid 33 flows. This electrode 2
Reference numeral 3 is for measuring the electric resistance value of the liquid flowing in the sheath flow cell 7, and a constant current is constantly applied between the electrodes by a constant current source 25 so that the particles are detected in the detection hole portion 22.
The inter-electrode voltage that changes as it passes through is measured. This inter-electrode voltage is taken out as the electric resistance detection signal 17 and processed by the signal processing unit described later.
【００３４】廃液チャンバ８は、測定の終わった液体を
回収する容器であり、粒子懸濁液の吸引にも用いられ
る。サンプル送出シリンジ９は、粒子懸濁液吸収ライン
に取り出された粒子懸濁液をシースフローセル７のサン
プルノズル２１へ送るための吸引を行うものである。な
お、図１には、溶液の吸引・送出に必要なバルブやフロ
ートスイッチ類は、装置の構成をわかりやすくするため
省略した。The waste liquid chamber 8 is a container for collecting the measured liquid and is also used for suctioning the particle suspension. The sample delivery syringe 9 carries out suction for sending the particle suspension taken out to the particle suspension absorption line to the sample nozzle 21 of the sheath flow cell 7. Note that, in FIG. 1, valves and float switches necessary for sucking / delivering the solution are omitted for the sake of easy understanding of the configuration of the apparatus.
【００３５】次に、図１の測定装置を用いたシースフロ
ー方式の電気的検知帯法の手順について説明する。
１）測定する粒子成分である粉体を導電性のある分散媒
（電解液）に懸濁させ、さらに粒子どうしの凝集を抑制
するための分散剤を添加、撹拌し、粒子懸濁液1 を作成
する。測定する粒子成分の例としては、微粒子、微生
物、生体細胞などがあり、これらの粒子成分を含む液体
試料の例として、血液、リンパ液、尿などの体液が挙げ
られる。また、分散剤としては、たとえば、ヘキタメタ
リン酸ソーダなどが用いられる。Next, the procedure of the sheath flow type electrical detection zone method using the measuring apparatus of FIG. 1 will be described. 1) Suspend the powder, which is the particle component to be measured, in a conductive dispersion medium (electrolytic solution), add a dispersant for suppressing the aggregation of the particles, and stir to prepare the particle suspension 1. create. Examples of particle components to be measured include fine particles, microorganisms, living cells, and the like, and examples of liquid samples containing these particle components include body fluids such as blood, lymph, and urine. Further, as the dispersant, for example, sodium hexametaphosphate or the like is used.
【００３６】２）溶液抽出用シリンジ４を吸収モードに
すること、具体的にはピストンを下げることによって、
粒子懸濁液１は吸引ピペット２を通ってフィルタユニッ
ト３に導かれ、懸濁液の溶液成分だけが溶液抽出用シリ
ンジ４に引き込まれる。
３）次に溶液抽出用シリンジ４を排出モードにする、具
体的にはピストンを上げることによって、抽出された溶
液は、溶液成分ライン１０を通ってシース液チャンバ６
に送られ貯められる。
４）次に排液チャンバ８を介して懸濁液吸引のための陰
圧（大気圧より低い圧力）をかけ、粒子懸濁液１を、フ
ィルタユニット３をそのまま通過させて粒子懸濁液吸引
ライン１１に引き込む。2) By putting the solution extracting syringe 4 in the absorption mode, specifically by lowering the piston,
The particle suspension 1 is guided to the filter unit 3 through the suction pipette 2, and only the solution component of the suspension is drawn into the solution extracting syringe 4. 3) Next, the extracted solution is passed through the solution component line 10 to bring the solution extraction syringe 4 into the discharge mode, specifically by raising the piston, and the sheath solution chamber 6
Sent to and stored. 4) Next, a negative pressure (pressure lower than atmospheric pressure) for suctioning the suspension is applied through the drainage chamber 8 to allow the particle suspension 1 to pass through the filter unit 3 as it is and suction the particle suspension. Pull into line 11.
【００３７】５）次にシース液チャンバ６に陽圧（大気
圧より高い圧力）をかけ、シース液チャンバ６内に貯め
られた抽出溶液をシース液としてシースフローセル７に
送出する。同時にサンプル送出リシンジ９を排出モード
にすることによって、粒子懸濁液１をシースフローセル
７のサンプルノズル２１に送り込む。また、シースフロ
ーセル７に供給されるシース液は、図２に示すようにフ
ロントシース液３２とバックシース液３３の２種類があ
る。5) Next, a positive pressure (higher than atmospheric pressure) is applied to the sheath liquid chamber 6, and the extraction solution stored in the sheath liquid chamber 6 is delivered to the sheath flow cell 7 as a sheath liquid. At the same time, the sample delivery reclining 9 is set to the discharge mode to feed the particle suspension 1 into the sample nozzle 21 of the sheath flow cell 7. As shown in FIG. 2, there are two types of sheath liquid supplied to the sheath flow cell 7, a front sheath liquid 32 and a back sheath liquid 33.
【００３８】６）サンプルノズルの先端から出てきた粒
子懸濁液流を、懸濁液から抽出された溶液（フロントシ
ース液３２）によって細かく絞り、検出孔部２２の細孔
２６を通過させる。
７）検出孔部２２の両側に設けられた電極の間に定電流
を流しておくことによって、粒子が細孔２６を通過する
時の電極間電圧を検出する。
８）検出孔部２２を通過してきた粒子懸濁液流は、懸濁
液から抽出された溶液（バックシース液３３）の働きに
よって回収管に取り込まれ、排液チャンバ８へ排出され
る。6) The particle suspension flow emerging from the tip of the sample nozzle is finely squeezed by the solution (front sheath liquid 32) extracted from the suspension, and passed through the fine holes 26 of the detection hole portion 22. 7) By passing a constant current between the electrodes provided on both sides of the detection hole portion 22, the inter-electrode voltage when the particles pass through the pores 26 is detected. 8) The particle suspension flow that has passed through the detection hole portion 22 is taken into the recovery pipe by the action of the solution (back sheath liquid 33) extracted from the suspension, and is discharged to the drainage chamber 8.
【００３９】以上のように粒子懸濁液から抽出した溶液
成分をシース液として利用すれば、粒子懸濁液流を細く
絞り込むためのシース液の電気伝導度は、懸濁液流の電
気導電度と一致する。従って、懸濁液とシース液のそれ
ぞれの電気伝導度が異なる場合に問題となる検出信号の
ゆらぎは発生しない。また、前記したような粒径と懸濁
液流の太さの関係で生じる粒径測定誤差も生じることは
ない。When the solution component extracted from the particle suspension is used as the sheath liquid as described above, the electric conductivity of the sheath liquid for narrowing down the particle suspension flow is as follows. Matches Therefore, the fluctuation of the detection signal, which is a problem when the electric conductivity of the suspension liquid and the electric conductivity of the sheath liquid are different, does not occur. Further, the particle size measurement error caused by the relationship between the particle size and the thickness of the suspension flow as described above does not occur.
【００４０】次に、測定される電極間電圧信号の変化量
を信号処理して粒子体積に相当するように補正する実施
例について説明する。粒子懸濁液の電気伝導度は、添加
される分散剤、温度等の違いにより異なることがある。
これは、同じ大きさの粒子が細孔２６を通過したとして
も、定電流を流している電極間の電圧変化量は同じでな
い場合があることを意味する。Next, an embodiment will be described in which the amount of change in the measured inter-electrode voltage signal is signal-processed and corrected so as to correspond to the particle volume. The electrical conductivity of the particle suspension may differ depending on the added dispersant, temperature, and the like.
This means that even if particles of the same size pass through the pores 26, the amount of voltage change between the electrodes that are flowing a constant current may not be the same.
【００４１】一方、電気伝導度が高いほど電極間の抵抗
値は小さくなる。従って、粒子が細孔２６を通過してい
ない時の電極間電圧（ＤＣ電圧）は、電気伝導度が高い
ほど小さく、粒子が細孔２６を通過する時の電極間電圧
の電圧変化量も電気伝導度が高いほど小さくなる。On the other hand, the higher the electric conductivity, the smaller the resistance value between the electrodes. Therefore, the inter-electrode voltage (DC voltage) when the particles are not passing through the pores 26 is smaller as the electric conductivity is higher, and the voltage change amount of the inter-electrode voltage when the particles are passing through the pores 26 is also electric. The higher the conductivity, the smaller.
【００４２】すなわち、粒子懸濁液の電気伝導度がある
程度大きい場合の電極間電圧変化量は電気伝導度に反比
例し、定電流値に比例する関係となる。また、電気伝導
度が非常に小さい場合には、電極間の電解液以外の経路
での微小電流の影響や定電流源の内部抵抗を無視できな
くなり、電極間電圧と電気伝導度とは正確に反比例しな
くなる。That is, when the electric conductivity of the particle suspension is large to some extent, the amount of change in voltage between electrodes is inversely proportional to the electric conductivity and proportional to the constant current value. Also, when the electric conductivity is very small, the influence of minute current in the path other than the electrolytic solution between the electrodes and the internal resistance of the constant current source cannot be ignored, and the voltage between the electrodes and the electric conductivity cannot be accurately measured. It will not be inversely proportional.
【００４３】ただし、粒子が細孔２６を通過する時の電
極間電圧の変化量は、粒子が細孔２６を通過していない
時の電極間電圧（ＤＣ電圧）と比例する。従って、粒子
通過による電極間電圧の電圧変化量を電極間ＤＣ電圧に
反比例させて補正すれば、粒子の体積に相当した正しい
電圧変化量が求められる。However, the amount of change in the inter-electrode voltage when the particles pass through the pores 26 is proportional to the inter-electrode voltage (DC voltage) when the particles do not pass through the pores 26. Therefore, if the voltage change amount of the inter-electrode voltage due to passage of particles is inversely proportional to the inter-electrode DC voltage and corrected, the correct voltage change amount corresponding to the volume of the particle can be obtained.
【００４４】また、懸濁液の電気伝導度の違いは、定電
流を流している電極間のＤＣ電圧を計測することによっ
て知ることができる。したがって粒子が細孔２６を通過
する時の電極間電圧変化量を、このＤＣ電圧レベルによ
って補正することにより、測定試料ごとに粒子懸濁液の
導電度が異なっても、ほぼ正しく粒子の大きさを求める
ことができる。このような補正をするための信号処理の
実施例を図４、図５に示す。Further, the difference in the electric conductivity of the suspension can be known by measuring the DC voltage between the electrodes passing a constant current. Therefore, by correcting the inter-electrode voltage change amount when the particles pass through the pores 26 by this DC voltage level, even if the conductivity of the particle suspension is different for each measurement sample, the particle size is almost correct. Can be asked. An embodiment of signal processing for making such a correction is shown in FIGS.
【００４５】図４の第１実施例において、電極間の電圧
変化を示す抵抗検出信号１７は低域通過フィルタ５１を
通り、その電圧レベルがサンプルホルダー５２で保持さ
れる。これは、粒子懸濁液の電気伝導度を反映するＤＣ
レベルの信号であり、後述する電圧制御増幅器５４の増
幅率を可変する信号として用いる。In the first embodiment of FIG. 4, the resistance detection signal 17 indicating the voltage change between the electrodes passes through the low pass filter 51, and the voltage level thereof is held by the sample holder 52. This is a DC that reflects the electrical conductivity of the particle suspension.
It is a level signal and is used as a signal for varying the amplification factor of the voltage control amplifier 54 described later.
【００４６】また、抵抗検出信号１７は高域通過フィル
タ５３を通過させられ、電圧制御増幅器５４に入力され
る。この入力される信号は、粒子の細孔通過による電極
間の電圧変化を表しており、その信号の振幅が、前記し
たＤＣレベル信号の大きさによって決められる増幅率で
もって電圧制御増幅器５４で増幅される。ここで、懸濁
液の電気伝導度が低い場合、すなわちＤＣレベル信号の
大きい場合ほど、増幅率は小さく設定される。The resistance detection signal 17 is passed through the high pass filter 53 and input to the voltage control amplifier 54. This input signal represents the voltage change between the electrodes due to the passage of particles through the pores, and the amplitude of the signal is amplified by the voltage control amplifier 54 with the amplification factor determined by the magnitude of the DC level signal. To be done. Here, when the electric conductivity of the suspension is low, that is, when the DC level signal is large, the amplification factor is set to be small.
【００４７】図６に抵抗検出信号のＤＣレベル信号とこ
の電圧制御増幅器５４の増幅率に対応する電圧変化信号
パルス高さの補正量との関係を示す。この増幅率すなわ
ち図６に示す補正量を決定するためには、あらかじめ何
種類かの大きさのそろった粒子を、粒子懸濁液の電気伝
導度を変化させながら測定し、その時の電極間のＤＣ電
圧及び電圧変化量を計測しておく。FIG. 6 shows the relationship between the DC level signal of the resistance detection signal and the correction amount of the voltage change signal pulse height corresponding to the amplification factor of the voltage control amplifier 54. In order to determine this amplification factor, that is, the correction amount shown in FIG. 6, particles of several kinds of sizes are previously measured while changing the electrical conductivity of the particle suspension, and the inter-electrodes at that time are measured. The DC voltage and the voltage change amount are measured.
【００４８】このように、ＤＣレベル信号１８に応じて
増幅された検出信号は、ＤＣ再生（５５）された上でそ
の信号パルスの高さがピークホルダー５６によって保持
される。さらに、その信号レベルをＡ／Ｄ変換（５７）
することにより、粒子の体積を反映する電圧変化信号パ
ルスの高さ情報１９が得られ、この情報はマイクロコン
ビュータ５８に取り込まれて粒度分布解析に利用され
る。なお、ＤＣ再生とは、抵抗検出信号のベースレベル
が０Ｖとなるようにすることである。As described above, the detection signal amplified in accordance with the DC level signal 18 is DC reproduced (55), and the height of the signal pulse is held by the peak holder 56. Further, the signal level is A / D converted (57).
By doing so, the height information 19 of the voltage change signal pulse that reflects the volume of the particle is obtained, and this information is taken into the micro-computer 58 and used for particle size distribution analysis. The DC reproduction means that the base level of the resistance detection signal becomes 0V.
【００４９】図５に、抵抗検出信号の信号処理の第２の
実施例を示す。ここでは、低域通過フィルタ５１とサン
プルホルダー５２によって得られたＤＣレベル信号をＡ
／Ｄ変換５９し、そのデータをマイクロコンピュータに
よってメモリ６０に取り込む。FIG. 5 shows a second embodiment of the signal processing of the resistance detection signal. Here, the DC level signal obtained by the low pass filter 51 and the sample holder 52 is
A / D conversion 59 is performed, and the data is taken into the memory 60 by the microcomputer.
【００５０】また、抵抗検出信号１７は、図４の第１実
施例のようにアナログ信号の段階で補正せずに、直接、
コンデンサ６１、ＤＣ再生５５、ピークホルダー５６を
通過させ、さらにＡ／Ｄ変換５７されて電圧変化信号パ
ルスの高さ情報としてマイクロコンピュータ５８によっ
てメモリ６０に記憶させられる。The resistance detection signal 17 is directly corrected without being corrected at the stage of the analog signal as in the first embodiment of FIG.
After passing through the capacitor 61, the DC regeneration 55 and the peak holder 56, the signal is A / D converted 57 and stored in the memory 60 by the microcomputer 58 as height information of the voltage change signal pulse.
【００５１】マイクロコンピュータ５８は、プログラム
処理によって、パルス高さ情報を先のＤＣレベル情報に
よって補正し、さらに個々の粒子体積あるいは体積相当
径を求める。The microcomputer 58 corrects the pulse height information with the above DC level information by program processing, and further obtains individual particle volume or volume equivalent diameter.
【００５２】体積相当径を求めるためには、図７に示す
ような補正後のパルス高さと体積相当径との関係をあら
かじめ求めておく必要がある。これは、図６の関係を導
くときに行ったのと同様の測定、すなわち何種類かの大
きさのそろった粒子を用いて電極間のＤＣ電圧と電圧変
化量を計測することによって求めることができる。In order to obtain the volume equivalent diameter, it is necessary to previously obtain the relationship between the corrected pulse height and the volume equivalent diameter as shown in FIG. This can be obtained by the same measurement as performed when deriving the relationship of FIG. 6, that is, by measuring the DC voltage between electrodes and the amount of voltage change using particles of several kinds of sizes. it can.
【００５３】図５に示した第２実施例では、あらかじめ
計測しておいた図６及び図７の関係をプログラムしてコ
ンピュータ５８に記憶しておくことにより、コンピュー
タ５８が入力される抵抗検出信号を自動的に補正して粒
子の体積相当径を求めることができる。In the second embodiment shown in FIG. 5, the resistance detection signal input to the computer 58 is programmed by programming the relationship of FIGS. 6 and 7 measured in advance and storing it in the computer 58. Can be automatically corrected to obtain the volume equivalent diameter of the particles.
【００５４】また、図２に示したシースフローセルにお
いて、前記したように検出孔部２２とその上部及び下部
が分解できる構造になっているが、これは孔のサイズの
異なる何種類かの検出孔部２２を容易に付け替えできる
ものである。このようなシースフローセルの構造にする
ことによって、シースフロー方式の電気的検知帯法で
も、粒径測定レンジの広い粒度分布測定装置を実現する
ことができる。Further, in the sheath flow cell shown in FIG. 2, the detection hole portion 22 and the upper and lower portions thereof can be disassembled as described above. This is because several kinds of detection holes having different hole sizes are used. The part 22 can be easily replaced. By adopting such a sheath flow cell structure, it is possible to realize a particle size distribution measuring device having a wide particle size measuring range even in the sheath flow type electrical detection zone method.
【００５５】ただし、検出孔部２２の孔径が異なると電
極間の抵抗に違いが生じ、同じ導電度の懸濁液で同じ値
の定電流を流しても電極間電圧は異なる。このような場
合には、ある基準の導電度の懸濁液を流し、その時の電
極間ＤＣ電圧が、ある基準の電圧値になるように定電流
値を可変できるようにしておくのが好ましい。また、図
６に示すように、検出孔部２２の孔のサイズごとにパル
ス高さと体積相当径の関係を前もって求めておく必要が
ある。However, if the hole diameter of the detection hole portion 22 is different, the resistance between the electrodes is different, and the voltage between the electrodes is different even if a constant current of the same value is flowed in a suspension having the same conductivity. In such a case, it is preferable that a suspension having a certain reference conductivity is flowed, and the constant current value can be changed so that the DC voltage between the electrodes at that time becomes a certain reference voltage value. Further, as shown in FIG. 6, it is necessary to previously obtain the relationship between the pulse height and the volume-equivalent diameter for each hole size of the detection hole portion 22.
【００５６】[0056]
【発明の効果】この発明によれば、被検出粒子を含む試
料液から溶液成分のみを抽出して、これをシース液とし
て測定手段に供給しているので、試料液とシース液の電
気伝導度が異なることのないようにでき正しく粒度分布
を測定することができる。また、測定手段の後室にシー
ス液を供給するので、検出孔部を通過した粒子の舞い戻
りを防ぐことができる。According to the present invention, since only the solution component is extracted from the sample liquid containing the particles to be detected and supplied as the sheath liquid to the measuring means, the electrical conductivity of the sample liquid and the sheath liquid is high. The particle size distribution can be measured correctly so that they do not differ. Further, since the sheath liquid is supplied to the rear chamber of the measuring means, it is possible to prevent the particles that have passed through the detection hole from returning.
【００５７】また、被検出粒子が検出孔部を通過する際
に生じる電気的信号のＤＣ成分レベル信号を検出してい
るので、懸濁液の電気伝導度が異なる場合でも、測定す
る粒子の大きさが正しく検出できるように電気的信号の
高さを補正できる。Since the DC component level signal of the electric signal generated when the particles to be detected pass through the detection hole portion is detected, the size of the particle to be measured is measured even if the electric conductivity of the suspension is different. The height of the electrical signal can be corrected so that the height can be detected correctly.
【００５８】また、前記測定装置の検出孔部が前室及び
後室と分離できる構造を持つため、検出孔部を孔径の異
なる細孔を持つ他の検出孔部と交換することができ、種
々の大きさを持つ粒子の粒度分布を測定することが可能
である。Further, since the detection hole portion of the measuring device has a structure that can be separated from the front chamber and the rear chamber, the detection hole portion can be replaced with another detection hole portion having pores having different hole diameters, It is possible to measure the particle size distribution of particles having a size of.
【図１】この発明の一実施例における粒度分布測定装置
の構成ブロック図である。FIG. 1 is a configuration block diagram of a particle size distribution measuring apparatus according to an embodiment of the present invention.
【図２】この発明の一実施例におけるシースフローセル
を示す模式図である。FIG. 2 is a schematic diagram showing a sheath flow cell in one embodiment of the present invention.
【図３】この発明の一実施例におけるフィルタユニット
の構成図である。FIG. 3 is a configuration diagram of a filter unit according to an embodiment of the present invention.
【図４】この発明の補正の信号処理における第１実施例
の構成ブロック図である。FIG. 4 is a configuration block diagram of a first embodiment in the signal processing for correction of the present invention.
【図５】この発明の補正の信号処理における第２実施例
の構成ブロック図である。FIG. 5 is a configuration block diagram of a second embodiment in the correction signal processing of the present invention.
【図６】この発明における検出信号パルス高さの補正例
を示すグラフである。FIG. 6 is a graph showing an example of correction of the detection signal pulse height according to the present invention.
【図７】この発明の検出信号パルス高さと粒子の体積相
当径の関係を示すグラフである。FIG. 7 is a graph showing the relationship between the detection signal pulse height and the volume equivalent diameter of particles according to the present invention.
１ 粒子懸濁液 ２ 吸引ピペット ３ フィルタユニット ４ 溶液抽出用シリンジ ５ 空圧源 ６ シース液チャンバ ７ シースフローセル ８ 廃液チャンバ ９ サンプル送出シリンジ １０ 溶液成分ライン １１ 粒子懸濁液吸収ライン １６ 懸濁液吸引圧 １７ 電気抵抗検出信号 ２１ サンプルノズル ２２ 検出孔部 ２３ 電極 ２４ 回収管 ２５ 定電流源 ２６ 細孔 ３１ 粒子懸濁液 ３２ フロントシース液 ３３ バックシース液 1 particle suspension 2 suction pipette 3 filter units 4 Solution extraction syringe 5 Air pressure source 6 Sheath liquid chamber 7 Sheath flow cell 8 waste liquid chamber 9 Sample delivery syringe 10 Solution component line 11 Particle suspension absorption line 16 Suspension suction pressure 17 Electric resistance detection signal 21 sample nozzle 22 Detection hole 23 electrodes 24 Collection pipe 25 constant current source 26 pores 31 particle suspension 32 Front sheath liquid 33 Back sheath liquid
Claims (7)
攪拌することによって試料液を調製する工程と、 前記試料液を吸引する工程と、 前記試料液から被検出粒子を除き溶液成分のみを抽出し
てシース液を調製する工程と、 被検出粒子を検出するための検出孔部と、前記試料液を
検出孔部に導く前室と、検出孔部から流出した前記試料
液を排出する後室とを備える測定手段に、前記試料液及
びシース液を導く工程と、 被検出粒子が前記検出孔部を通過する際の電気抵抗の変
化を電気信号として検知する工程と、 電気信号に基づいて粒度分布を得る工程と、からなる粒
度分布測定方法。 1. A detection target particle, a conductive dispersion medium, and a dispersant.
A step of preparing a sample solution by stirring, a step of sucking the sample solution , and removing only particles to be detected from the sample solution to extract only a solution component
To prepare the sheath liquid, the detection hole for detecting the particles to be detected , and the sample liquid.
The front chamber leading to the detection hole and the sample flowing out from the detection hole
The sample solution and the sample solution are added to the measuring means having a rear chamber for discharging the solution.
And the process of introducing the sheath liquid, and the change in the electrical resistance when the particles to be detected pass through the detection hole.
Particle consisting of the step of detecting the aging as an electric signal and the step of obtaining a particle size distribution based on the electric signal.
Degree distribution measurement method.
る粒度分布測定装置において、被検出粒子と導電性分散
媒と分散剤とを含む試料液を収容する容器と、前記容器
から供給された被検出粒子を検出するための検出孔部
と、被検出粒子を含む試料液を検出孔部に導く前室と、
検出孔部から流出した前記試料液を排出する後室とを備
える測定手段と、 前記試料液から被検出粒子を除き溶液成分のみを抽出す
る溶液抽出手段と、 前記溶液抽出手段によって抽出される溶液成分をシース
液として前記測定手段に供給するシース液供給手段と、 被検出粒子が前記検出孔部を通過する際の電気抵抗の変
化を電気信号として検知する信号検知手段とを備えるこ
とを特徴とする粒度分布測定装置。2. A particle size distribution measuring apparatus using a sheath flow type electric detection zone method, wherein particles to be detected and conductive dispersion are present.
A container for containing a sample solution containing a medium and a dispersant, and the container
A detection hole portion for detecting the particles to be detected supplied from, and a front chamber for guiding the sample liquid containing the particles to be detected to the detection hole portion,
A measuring means having a rear chamber for discharging the sample solution flowing out from the detection hole portion, a solution extracting means for extracting only a solution component from the sample solution excluding particles to be detected, and a solution extracted by the solution extracting means A sheath liquid supply unit that supplies a component as a sheath liquid to the measurement unit, and a signal detection unit that detects a change in electric resistance when a particle to be detected passes through the detection hole as an electric signal. Particle size distribution measuring device.
の前室及び後室に前記シース液を供給することを特徴と
する請求項２記載の粒度分布測定装置。3. The particle size distribution measuring device according to claim 2, wherein the sheath liquid supplying means supplies the sheath liquid to the front chamber and the rear chamber of the measuring means.
備えることを特徴とする請求項２記載の粒度分布測定装
置。4. The particle size distribution measuring device according to claim 2 , wherein the solution extracting means includes a hollow fiber filter.
気信号のＤＣ成分を抽出し、このＤＣ成分信号を利用し
て前記電気信号のレベルを補正する補正手段を備え、前
記補正手段が被検出粒子の粒度分布に対応する測定信号
を生成することを特徴とする請求項２記載の粒度分布測
定装置。5. A extracts the DC component of the electrical signal detected by the signal detecting means, a correction means for correcting a level of the electrical signal by using the DC component signal, before <br/> SL correction The particle size distribution measuring apparatus according to claim 2 , wherein the means generates a measurement signal corresponding to the particle size distribution of the particles to be detected.
室及び後室に配置される一対の電極を備え、この電極間
の電圧に対応する電気信号を検知し、前記補正手段が前
記電気信号のＤＣ成分信号によって電気信号の増幅率を
調整することを特徴とする請求項５記載の粒度分析測定
装置。Wherein said signal detecting means, wherein a pair of electrodes disposed in the front chamber and the rear chamber of the measuring means, detects that electrostatic No. venlafaxine corresponding to the voltage between the electrodes, wherein the correction means the electrostatic connexin No. of granulometric measuring device according to claim 5, wherein the adjusting the gain of the No. conductive relaxin by DC component signal.
室と分離できる構造を有することを特徴とする請求項２
から請求項６のいずれかに記載した粒度分析測定装置。Detection hole according to claim 7, wherein said measuring device is characterized by having a structure capable of separating a front chamber and a rear chamber according to claim 2
7. The particle size analysis measuring device according to claim 6 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20987694A JP3499009B2 (en) | 1994-09-02 | 1994-09-02 | Particle size distribution analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20987694A JP3499009B2 (en) | 1994-09-02 | 1994-09-02 | Particle size distribution analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0875632A JPH0875632A (en) | 1996-03-22 |
| JP3499009B2 true JP3499009B2 (en) | 2004-02-23 |
Family
ID=16580114
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20987694A Expired - Fee Related JP3499009B2 (en) | 1994-09-02 | 1994-09-02 | Particle size distribution analyzer |
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| Country | Link |
|---|---|
| JP (1) | JP3499009B2 (en) |
Cited By (1)
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| WO2014023112A1 (en) * | 2012-08-10 | 2014-02-13 | 深圳迈瑞生物医疗电子股份有限公司 | Flow instrument and liquid path system |
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|---|---|---|---|---|
| JP3403564B2 (en) * | 1995-12-04 | 2003-05-06 | 日機装株式会社 | Powder particle size distribution analyzer |
| JP5629447B2 (en) * | 2009-10-07 | 2014-11-19 | 株式会社セイシン企業 | Particle property measuring method and apparatus, and measuring sample preparation apparatus |
| JP6208487B2 (en) * | 2013-07-22 | 2017-10-04 | 日本光電工業株式会社 | Blood measuring device |
| JP7315257B2 (en) * | 2019-10-11 | 2023-07-26 | アイポア株式会社 | Sensors, measuring instruments, computing devices and systems for particle identification |
| CN117740631B (en) * | 2024-02-19 | 2024-05-03 | 中国石油大学(华东) | Electrical signal scale sample for measuring emulsion particle size and scale method |
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1994
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014023112A1 (en) * | 2012-08-10 | 2014-02-13 | 深圳迈瑞生物医疗电子股份有限公司 | Flow instrument and liquid path system |
| US9170187B2 (en) | 2012-08-10 | 2015-10-27 | Shenzhen Mindray Bio-Medical Electronics Co., Ltd. | Flow cytometer and fluidic system thereof |
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| Publication number | Publication date |
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| JPH0875632A (en) | 1996-03-22 |
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