Deprecated: The each() function is deprecated. This message will be suppressed on further calls in /home/zhenxiangba/zhenxiangba.com/public_html/phproxy-improved-master/index.php on line 456
JP3552399B2 - Laser diffraction particle size distribution analyzer - Google Patents
[go: Go Back, main page]

JP3552399B2 - Laser diffraction particle size distribution analyzer - Google Patents

Laser diffraction particle size distribution analyzer Download PDF

Info

Publication number
JP3552399B2
JP3552399B2 JP08673896A JP8673896A JP3552399B2 JP 3552399 B2 JP3552399 B2 JP 3552399B2 JP 08673896 A JP08673896 A JP 08673896A JP 8673896 A JP8673896 A JP 8673896A JP 3552399 B2 JP3552399 B2 JP 3552399B2
Authority
JP
Japan
Prior art keywords
sample
cell
particle size
size distribution
laser diffraction
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
Application number
JP08673896A
Other languages
Japanese (ja)
Other versions
JPH09281026A (en
Inventor
和 竹内
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.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP08673896A priority Critical patent/JP3552399B2/en
Publication of JPH09281026A publication Critical patent/JPH09281026A/en
Application granted granted Critical
Publication of JP3552399B2 publication Critical patent/JP3552399B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Images

Landscapes

  • Optical Measuring Cells (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Description

【0001】
【発明の属する技術分野】
本発明は、少量かつ比較的高濃度のサンプルの粒度測定に用いられるレーザ回折式粒度分布測定装置に関する。
【0002】
【従来の技術】
レーザ回折式粒度分布測定装置では通常液体に懸濁させた粒子をレーザビームの照射位置を通過させて循環させるか、あるいは乾燥した粉体を圧縮空気により分散させ、レーザビーム中に吹き込むことにより、測定が行われており、少量の試料の場合はガラス製の箱型のセル中に液体に懸濁した粒子を入れ、それをレーザビーム照射位置に固定するという方法を取っている。
【0003】
液体に懸濁させた粒子を循環させる場合、ポンプ、液体の流路となるパイプ等が必要となり、構成が複雑になるとともに測定後試料粒子が残留し、次の測定に誤差を生じたり、洗浄が面倒である。
【0004】
一方、圧縮空気で粒子を分散させる方法でも圧縮空気源、分散した粒子を集める集塵器等が必要であり、さらに粒子が飛散するため回収が不可能であるとともに、多量の試料が必要であり、毒物性のものには向かない。箱型のセルは少量の試料で構成も簡単だが、液体に懸濁させねばならず、レーザビーム透過のための希釈も必要である。
【0005】
そこで、これらの欠点を解消するために開放型のセルに試料を入れ、これに対してレーザ光源を下方に配置して粒度分布を測定する方法が用いられている。
【0006】
従来、この方式のレーザ回折式粒度分布測定では、図4に示すように、サンプル(試料)Sを入れた試料セル101を、レーザ光通過孔102aを設けた設置台102上に置き、下方に設置されたレーザ光源103から、レーザ光を発射し、コリメータ104によって、所定断面積を持つ平行光束とした後、コリメータ104及びレーザ光源103保護用の透明カバー105を介して、試料101に直角に照射し上方から出る回折/散乱光を集光レンズ106で集光した後、リングデテクタ等の前方回折/散乱光センサ107によって検出し、サンプルSの粒度分布を測定している。
【0007】
【発明が解決しようとする課題】
ところで、上記の装置では構成が簡単であり、洗浄や測定試料の回収は容易に行えるものの、ペーストやスラリー等の高濃度のサンプルの粒度分布を測定する場合には、多重散乱光の発生を低減するために、レーザ光の光軸に対し、サンプルの厚さを極めて薄くする必要がある。
【0008】
しかし、上記従来技術では、適当な深さの開放型セルを用いているのでサンプル層の厚さを簡単に薄くすることが困難であり、特に、試料が乾燥粉体の場合にはサンプル層の厚さが部分的に異なり測定データがばらついていた。
【0009】
本発明は、上記課題を解決するために創案されたもので、乾燥状、液状の測定試料の種類を問わず簡単に薄いサンプル層をつくることができ、高濃度のサンプルであっても、多重散乱の発生を極めて少なくするとともに、サンプル層の厚さの不均一による測定データの誤差を少なくすることができるレーザ回折式粒度分布測定装置を提供するものである。
【0010】
【課題を解決するための手段】
上記目的を達成するために、本発明のレーザ回折式粒度分布測定装置は、サンプルを収容する試料セルと、試料セルにレーザ光を照射する手段と、レーザ光の照射により得られるサンプル粒子群による回折/散乱光の強度分布を測定する手段とを備えたレーザ回折式粒度分布測定装置において、前記試料セルが、透光性の平板状の板にサンプル粒子の大きさとほぼ等しい深さを持つ凹部を形成したものであることを特徴としている。
【0011】
レーザ光を試料に照射し、これにより発生する回折/散乱光の強度分布を測定することによって粒度分布を測定するが、試料はおよそ試料粒子の大きさと等しい深さを持つ試料セルに入れられるので、簡単に試料をセットすることができるとともに、高濃度の試料を測定する場合でも、乾燥状、液状の測定試料の種類を問わず、レーザ光の透過が保証され、多重散乱の発生を極めて少なくすることができるので、正確な測定ができる。
【0012】
【発明の実施の形態】
本発明の一実施例を、以下、図面に基づいて説明する。
【0013】
図1は本発明によるレーザ回折式粒度分布測定装置における試料セルを示す。
図1(a)はセルの平面図であり、(b)はセルの側面図である。
【0014】
1は平面状のガラス等の透光性の物質で構成されたセル、2はセル1に設けられた円形状の窪み2(凹部)である。この窪み2はセル1を貫通せずに底面にある程度(1mm程度)の厚さを残しておく。そして、窪み2の底面はレーザビームが通過する関係上散乱等を起こさないように光学研磨をほどこしておく。また、窪み2の底面の大きさはレーザビームの断面積よりは大きく形成されている。ところで、種々の深さのセルが用意されており、測定時にはサンプルの種類に応じて、これらのセルを選択する。この場合、あらかじめ粒子の大きさを予測し、窪み2の深さは試料の最大粒子径よりもやや深いものを使用する。
【0015】
この場合、試料が懸濁液であると、試料をセットした後にこのセルをレーザビームの照射位置に設置すれば良いが、試料が乾燥粉体であると、図2に示すようにセルの窪み2に乾燥粉体4を入れた後、プレート3でセル1の表面を擦り切って表面を平にするか、平板をセル1の窪み2の部分に押し当ててその表面を平にする必要がある。このようにすることによって、サンプル層の厚さを各部均一にすることができるとともに、粒子層が多層とならないために、多重散乱の発生を抑制することができる。
【0016】
なお、窪み2の形状は円形でなくても良いが、円形の方が側面に角がなく、試料測定前や、試料測定後のセルの掃除には便利である。
【0017】
次に、このようにして試料がセットされたセルを用いた粒度分布測定を行う方法を図4の装置により説明する。
【0018】
上記のようにサンプル(試料)を入れた試料セル1を、レーザ光通過孔102aを設けた設置台102上に置き、下方に設置されたレーザ光源103から、レーザ光を発射し、コリメータ104によって、所定断面積を持つ平行光束とした後、コリメータ104及びレーザ光源103保護用の透明カバー105を介して、試料101に直角に照射し、上方から出る回折/散乱光を集光レンズ106で集光した後、リングデテクタ等の前方回折/散乱光センサ107によって検出し、サンプルSの粒度分布測定を行う。
【0019】
この測定の時に、試料が懸濁液の場合には特にセル中の液面が水平になるように設置台102には水平調節機構が付いているのが望ましい。
【0020】
上述の実施例では、セルの窪みの形状はその底面が完全にフラットになるようにしたが、図3に示すように窪み(凹部)6の形状を球面状としても良い。この場合には、凹部の曲率半径が極めて大きければ、底面はフラットとみなせ、底面を完全にフラットにするよりも研磨による加工が容易であり、窪みの深さを粒子の大きさに等しいか、それに極めて近い深さ、すなわち10um程度に容易に加工できる。
【0021】
さらに、底面を球面状としているので、底面をフラットにしたときのような底面とこれに垂直な側面とで形成されるコーナー部分ができず、試料粒子が溜まらないので、セル5の清掃がよりいっそう簡単になる。
【0022】
また、平面状のセルの窪みの上に光学的な歪みのない薄いカバーガラスを置いても良く、このカバーガラスとセルとの間にシール剤を入れれば、レーザ光源、コリメータ、セル、レンズ、センサを水平においた横型のレーザ回折式粒度分布測定装置にも使用することができる。
【0023】
【発明の効果】
以上説明したように、本発明によれば、セルに凹部を設け、その窪みの深さを、測定試料の粒子の大きさとほぼ同じにしているので、乾燥状、液状の測定試料の種類を問わず簡単に薄いサンプル層をつくることができ、高濃度のサンプルであっても、多重散乱の発生を極めて少なくするとともに、サンプル層の厚さの不均一による測定データの誤差を少なくすることができる。
【図面の簡単な説明】
【図1】本発明のレーザ回折式粒度分布測定装置のセルを示す図である。
【図2】乾燥粉体をセルにセットする方法例を示す図である。
【図3】セルに異なる形状の窪みを設けた例を示す図である。
【図4】縦型のレーザ回折式粒度分布測定装置を示す図である。
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a laser diffraction type particle size distribution measuring device used for measuring the particle size of a sample having a relatively small concentration and a relatively high concentration.
[0002]
[Prior art]
In a laser diffraction type particle size distribution measuring device, particles suspended in a liquid are usually circulated through a laser beam irradiation position, or dried powder is dispersed by compressed air and blown into the laser beam, Measurement is performed. In the case of a small amount of sample, particles suspended in a liquid are placed in a glass box-shaped cell and fixed at the laser beam irradiation position.
[0003]
In the case of circulating particles suspended in liquid, a pump, pipes for liquid flow path, etc. are required, which complicates the configuration and causes sample particles to remain after measurement, causing errors in the next measurement or washing. Is troublesome.
[0004]
On the other hand, the method of dispersing particles with compressed air also requires a compressed air source, a dust collector that collects the dispersed particles, and the like. Not suitable for toxic substances. A box cell is simple to construct with a small amount of sample, but must be suspended in a liquid and requires dilution for laser beam transmission.
[0005]
In order to solve these drawbacks, a method has been used in which a sample is placed in an open cell, and a laser light source is disposed below the cell to measure the particle size distribution.
[0006]
Conventionally, in this type of laser diffraction type particle size distribution measurement, as shown in FIG. 4, a sample cell 101 containing a sample (sample) S is placed on an installation table 102 provided with a laser beam passage hole 102a, and Laser light is emitted from the installed laser light source 103, and is collimated by a collimator 104 into a parallel light beam having a predetermined cross-sectional area. After irradiating the diffracted / scattered light from above and condensing it with a condenser lens 106, the diffracted / scattered light is detected by a forward diffracted / scattered light sensor 107 such as a ring detector, and the particle size distribution of the sample S is measured.
[0007]
[Problems to be solved by the invention]
By the way, the above-described apparatus has a simple structure, and can easily wash and collect a measurement sample. However, when measuring the particle size distribution of a high-concentration sample such as a paste or a slurry, the occurrence of multiple scattered light is reduced. Therefore, it is necessary to make the thickness of the sample extremely thin with respect to the optical axis of the laser beam.
[0008]
However, in the above prior art, it is difficult to easily reduce the thickness of the sample layer because an open cell having an appropriate depth is used. The thickness was partially different, and the measurement data varied.
[0009]
The present invention has been made in order to solve the above-mentioned problems, and can easily form a thin sample layer regardless of the type of a dry or liquid measurement sample. An object of the present invention is to provide a laser diffraction type particle size distribution measuring apparatus capable of extremely reducing the occurrence of scattering and reducing errors in measurement data due to non-uniform thickness of a sample layer.
[0010]
[Means for Solving the Problems]
In order to achieve the above object, a laser diffraction type particle size distribution measuring apparatus according to the present invention comprises a sample cell containing a sample, a means for irradiating the sample cell with laser light, and a sample particle group obtained by irradiating the laser light. A laser diffraction type particle size distribution measuring apparatus provided with means for measuring the intensity distribution of diffraction / scattered light, wherein the sample cell has a concave portion having a depth substantially equal to the size of the sample particles in a translucent flat plate. Is formed.
[0011]
The particle size distribution is measured by irradiating the sample with laser light and measuring the intensity distribution of the resulting diffraction / scattered light. However, since the sample is placed in a sample cell having a depth approximately equal to the size of the sample particle, The sample can be easily set, and even when measuring a high-concentration sample, the transmission of laser light is guaranteed regardless of the type of the dry or liquid sample, and the occurrence of multiple scattering is extremely reduced. So that accurate measurements can be made.
[0012]
BEST MODE FOR CARRYING OUT THE INVENTION
An embodiment of the present invention will be described below with reference to the drawings.
[0013]
FIG. 1 shows a sample cell in a laser diffraction type particle size distribution measuring apparatus according to the present invention.
FIG. 1A is a plan view of a cell, and FIG. 1B is a side view of the cell.
[0014]
Reference numeral 1 denotes a cell formed of a light-transmitting substance such as a flat glass, and 2 denotes a circular depression 2 (recess) provided in the cell 1. The recess 2 does not penetrate the cell 1 and has a certain thickness (about 1 mm) on the bottom surface. Then, the bottom surface of the depression 2 is optically polished so as not to cause scattering or the like due to the passage of the laser beam. The size of the bottom surface of the depression 2 is formed larger than the cross-sectional area of the laser beam. By the way, cells of various depths are prepared, and these cells are selected at the time of measurement according to the type of sample. In this case, the size of the particle is predicted in advance, and the depth of the depression 2 is slightly larger than the maximum particle diameter of the sample.
[0015]
In this case, if the sample is a suspension, the cell may be set at the irradiation position of the laser beam after setting the sample. However, if the sample is a dry powder, the cell is recessed as shown in FIG. After putting the dry powder 4 into the plate 2, the surface of the cell 1 must be flattened by scraping the surface of the cell 1 with the plate 3, or the plate must be pressed against the recess 2 of the cell 1 to flatten the surface. is there. By doing so, the thickness of the sample layer can be made uniform in each part, and the occurrence of multiple scattering can be suppressed because the particle layer does not have multiple layers.
[0016]
The shape of the depression 2 does not have to be circular, but the circular shape has no corners on the side surface and is more convenient for cleaning cells before and after sample measurement.
[0017]
Next, a method of measuring the particle size distribution using the cell in which the sample is set as described above will be described using the apparatus shown in FIG.
[0018]
The sample cell 1 in which the sample (sample) is placed as described above is placed on the mounting table 102 provided with the laser light passage hole 102a, and the laser light is emitted from the laser light source 103 installed below, and the collimator 104 emits the laser light. After being converted into a parallel light beam having a predetermined sectional area, the sample 101 is irradiated at right angles to the sample 101 via a collimator 104 and a transparent cover 105 for protecting the laser light source 103, and diffracted / scattered light emitted from above is collected by a condenser lens 106. After the light emission, the light is detected by a forward diffraction / scattered light sensor 107 such as a ring detector, and the particle size distribution of the sample S is measured.
[0019]
At the time of this measurement, when the sample is a suspension, it is desirable that the installation table 102 be provided with a horizontal adjustment mechanism so that the liquid level in the cell is particularly horizontal.
[0020]
In the above-described embodiment, the shape of the dent of the cell is such that the bottom surface is completely flat. However, the shape of the dent (recess) 6 may be spherical as shown in FIG. In this case, if the radius of curvature of the concave portion is extremely large, the bottom surface can be regarded as flat, processing by polishing is easier than making the bottom surface completely flat, and the depth of the depression is equal to the size of the particle, It can be easily processed to a depth very close to that, that is, about 10 μm.
[0021]
Furthermore, since the bottom surface is spherical, there is no corner portion formed by the bottom surface and the side surface perpendicular to the bottom surface as when the bottom surface is flat, and the sample particles do not accumulate. It gets even easier.
[0022]
Also, a thin cover glass without optical distortion may be placed on the recess of the planar cell, and if a sealant is put between the cover glass and the cell, a laser light source, a collimator, a cell, a lens, The present invention can also be used for a horizontal laser diffraction type particle size distribution measuring device in which a sensor is placed horizontally.
[0023]
【The invention's effect】
As described above, according to the present invention, since the concave portion is provided in the cell and the depth of the concave portion is made substantially the same as the size of the particles of the measurement sample, the type of the dry or liquid measurement sample can be determined. It is possible to easily create a thin sample layer, and to minimize the occurrence of multiple scattering, even for a sample with a high concentration, and to reduce errors in measurement data due to uneven thickness of the sample layer. .
[Brief description of the drawings]
FIG. 1 is a view showing a cell of a laser diffraction type particle size distribution measuring apparatus of the present invention.
FIG. 2 is a diagram showing an example of a method for setting a dry powder in a cell.
FIG. 3 is a diagram showing an example in which a dent having a different shape is provided in a cell.
FIG. 4 is a view showing a vertical laser diffraction type particle size distribution measuring device.

Claims (1)

サンプルを収容する試料セルと、試料セルにレーザ光を照射する手段と、レーザ光の照射により得られるサンプル粒子群による回折/散乱光の強度分布を測定する手段とを備えたレーザ回折式粒度分布測定装置において、前記試料セルが、透光性の平板状の板にサンプル粒子の大きさとほぼ等しい深さを持つ凹部を形成したものであることを特徴とするレーザ回折式粒度分布測定装置。A laser diffraction particle size distribution comprising a sample cell for accommodating a sample, a means for irradiating the sample cell with laser light, and a means for measuring the intensity distribution of diffraction / scattered light by the sample particle group obtained by the laser light irradiation In a measuring apparatus, the sample cell is formed by forming a concave portion having a depth substantially equal to the size of a sample particle on a light-transmitting flat plate-shaped plate, wherein a laser diffraction type particle size distribution measuring apparatus is used.
JP08673896A 1996-04-09 1996-04-09 Laser diffraction particle size distribution analyzer Expired - Fee Related JP3552399B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP08673896A JP3552399B2 (en) 1996-04-09 1996-04-09 Laser diffraction particle size distribution analyzer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP08673896A JP3552399B2 (en) 1996-04-09 1996-04-09 Laser diffraction particle size distribution analyzer

Publications (2)

Publication Number Publication Date
JPH09281026A JPH09281026A (en) 1997-10-31
JP3552399B2 true JP3552399B2 (en) 2004-08-11

Family

ID=13895164

Family Applications (1)

Application Number Title Priority Date Filing Date
JP08673896A Expired - Fee Related JP3552399B2 (en) 1996-04-09 1996-04-09 Laser diffraction particle size distribution analyzer

Country Status (1)

Country Link
JP (1) JP3552399B2 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5533748B2 (en) * 2011-03-16 2014-06-25 トヨタ自動車株式会社 Particle size measuring method and particle size measuring device

Also Published As

Publication number Publication date
JPH09281026A (en) 1997-10-31

Similar Documents

Publication Publication Date Title
JP3936220B2 (en) Edge inspection equipment
JP2996193B2 (en) Wafer inspection method and apparatus
JP3552399B2 (en) Laser diffraction particle size distribution analyzer
JPH0933423A (en) Vertical laser diffraction particle size distribution analyzer
JPH0787208B2 (en) Face plate defect detection optical device
US6108077A (en) Sample support with a non-reflecting sample supporting surface
JP2004170320A (en) Particle size distribution measuring apparatus
JP3989836B2 (en) Sample condition inspection apparatus and method
JPH0933435A (en) Device for measuring optical characteristic value of transparent material
US5453830A (en) Spatially isolated diffractor on a calibration substrate for a pellicle inspection system
WO1991014935A1 (en) A method and an apparatus for cleaning control
JPS5599049A (en) Defect detector
EP4139658A1 (en) A spacer for a cuvette, use thereof and a method of analysing a sample
JP3301049B2 (en) Gas analyzer using ultraviolet fluorescence analysis
CN223400351U (en) A device for quickly measuring wafer roughness
CN220084691U (en) Optical measuring device
JP2948353B2 (en) Glass plate surface defect inspection method and inspection device
JP3160234U (en) Sample cell and particle size distribution measuring apparatus using the same
JPH0431748A (en) Defect inspecting method for transparent plate-shaped body
JPH04249761A (en) Apparatus for inspecting foreign matter
JPH01110349U (en)
JPS6321854B2 (en)
JPH1090158A (en) Apparatus for measuring concentration and grain size of air-borne particles
Brun et al. Reflection spectroscopy in microstructured light scattering materials
JP3025051B2 (en) Scattered light measurement cell

Legal Events

Date Code Title Description
A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20040206

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20040413

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20040426

R150 Certificate of patent or registration of utility model

Free format text: JAPANESE INTERMEDIATE CODE: R150

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20080514

Year of fee payment: 4

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20090514

Year of fee payment: 5

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100514

Year of fee payment: 6

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100514

Year of fee payment: 6

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110514

Year of fee payment: 7

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110514

Year of fee payment: 7

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120514

Year of fee payment: 8

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130514

Year of fee payment: 9

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130514

Year of fee payment: 9

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20140514

Year of fee payment: 10

LAPS Cancellation because of no payment of annual fees