JPH047828B2 - - Google Patents
Info
- Publication number
- JPH047828B2 JPH047828B2 JP10698484A JP10698484A JPH047828B2 JP H047828 B2 JPH047828 B2 JP H047828B2 JP 10698484 A JP10698484 A JP 10698484A JP 10698484 A JP10698484 A JP 10698484A JP H047828 B2 JPH047828 B2 JP H047828B2
- Authority
- JP
- Japan
- Prior art keywords
- light
- slit
- light source
- optical cell
- slits
- 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
Links
- 230000003287 optical effect Effects 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 10
- 238000006073 displacement reaction Methods 0.000 claims description 7
- 238000005192 partition Methods 0.000 claims description 5
- 230000035945 sensitivity Effects 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000004454 trace mineral analysis Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000010206 sensitivity analysis Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/4133—Refractometers, e.g. differential
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【発明の詳細な説明】
(イ) 目的
（産業上の利用分野）
本発明は液体クロマトグラフの検出器などにお
いて、透明な液体間に生じる屈折率の差を光学的
に検出する装置に関するものである。[Detailed Description of the Invention] (a) Purpose (Field of Industrial Application) The present invention relates to a device for optically detecting the difference in refractive index that occurs between transparent liquids, such as in a liquid chromatograph detector. be.
（従来の技術）
高速液体クロマトグラフの検出器として示差屈
折計検出器が用いられるが、その用途としては微
量分析用の高感度示差屈折計と、分取用の低感度
示差屈折計がある。これらは通常別個の製品とし
て製品化されている。(Prior Art) A differential refractometer detector is used as a detector in a high-performance liquid chromatograph, and its applications include a high-sensitivity differential refractometer for trace analysis and a low-sensitivity differential refractometer for preparative separation. These are usually commercialized as separate products.
また、光学セルの２個の容器を分離する隔壁に
対する光の入射角度の大きさにより感度が変化す
るところから、隔壁の角度の異なる光学セルに交
換することにより用途に応じた感度を得るように
する場合もある。 In addition, since the sensitivity changes depending on the angle of incidence of light on the partition wall that separates the two containers of the optical cell, it is possible to obtain sensitivity according to the application by replacing the optical cell with an optical cell with a different partition wall angle. In some cases.
（発明が解決しようとする問題点）
用途に応じて感度を変えるために、光学セルを
交換し、調整したりすることは、厄介な作業であ
る。(Problems to be Solved by the Invention) It is a troublesome task to replace and adjust the optical cell in order to change the sensitivity depending on the application.
本発明は、１個の装置で、しかも簡単な切替え
操作により感度とリニアリテイレンジの範囲を同
時に増減させ、高感度な微量分析用と、低感度な
分取用の２つの用途に使える示差屈折計を提供す
ることを目的とするものである。 The present invention is a differential refraction system that can simultaneously increase and decrease the sensitivity and linearity range with a single device and a simple switching operation, and can be used for two purposes: high-sensitivity trace analysis and low-sensitivity preparative separation. The purpose is to provide a
(ロ) 構成
（問題点を解決するための手段）
本発明は光の入射方向に対し傾斜した隔壁で分
離された２個の容器を有する光学セルに光を入射
し、両容器内の液体の屈折率差に対応した透過光
の変位を測定する示差屈折計において、
スリツト幅の異なる２種類のスリツトと、
光学セルへ入射される光の光源の光量を制御す
る手段と、を備え、
スリツトの切替えと同時に光源の光量をスリツ
ト幅に反比例するように変化させるようにした示
差屈折計である。(B) Configuration (Means for solving the problem) The present invention involves injecting light into an optical cell having two containers separated by a partition wall that is inclined with respect to the direction of light incidence, and measuring the amount of liquid in both containers. A differential refractometer that measures the displacement of transmitted light corresponding to the difference in refractive index is equipped with two types of slits with different widths, and a means for controlling the amount of light from a light source that enters the optical cell, This is a differential refractometer that changes the light intensity of the light source in inverse proportion to the slit width at the same time as switching.
（作用）
第２図に示される光センサ２が測定光の変位方
向に２個の部分に分けられているとする。一方を
Ｓ側２−１、他方をＲ側２−２とする。光学セル
の２個の容器の液体に屈折率差がないときには２
個の光センサ２−１，２−２の中央にｄ×ａの面
積のスリツト像の光が入射する。ｄはスリツト幅
に対応し、ａはスリツトの長さに対応する。 次
に２個の容器の液体間の屈折率がΔnだけ変化し
たとすると、その屈折率差Δnに応じて光センサ
２上のスリツトの像がΔdだけ変位し、この変位
量は
ｌ・Δn／ｎ
に比例する。ｌは光学セルと光センサ２との距
離、ｎは溶媒の屈折率である。(Operation) It is assumed that the optical sensor 2 shown in FIG. 2 is divided into two parts in the displacement direction of the measurement light. One side is S side 2-1 and the other side is R side 2-2. 2 when there is no difference in refractive index between the liquids in the two containers of the optical cell.
Light from a slit image having an area of d×a enters the center of each of the optical sensors 2-1 and 2-2. d corresponds to the slit width, and a corresponds to the slit length. Next, if the refractive index between the liquids in the two containers changes by Δn, the image of the slit on the optical sensor 2 will be displaced by Δd in accordance with the refractive index difference Δn, and this amount of displacement will be l・Δn/ Proportional to n. l is the distance between the optical cell and the optical sensor 2, and n is the refractive index of the solvent.
光センサ２上の光強度をＩとすると、Ｓ側光セ
ンサ２−１、Ｒ側光センサ２−２のそれぞれに現
れる信号is，irは、それぞれ
〔（ｄ／２）＋Δd〕Ia ……(1)
〔（ｄ／２）−Δd〕Ia ……(2)
に比例する。 If the light intensity on the optical sensor 2 is I, the signals is and ir appearing on the S-side optical sensor 2-1 and the R-side optical sensor 2-2 are respectively [(d/2)+Δd]Ia...( 1) Proportional to [(d/2)-Δd]Ia...(2).
本発明において、スリツト幅をＭ倍とし、光源
の光量を１／Ｍとすると、ｄ→Md，Ｉ→Ｉ／Ｍ
となるため、(1)，(2)式において、Δdを含まない
定常項は不変であるが、屈折率差Δnに対応する
変位Δdによる信号、すなわち感度はΔd・Ia／Ｍ
となり、１／Ｍに低下する。 In the present invention, if the slit width is multiplied by M and the light intensity of the light source is set to 1/M, then d→Md, I→I/M
Therefore, in equations (1) and (2), the stationary term that does not include Δd remains unchanged, but the signal due to the displacement Δd corresponding to the refractive index difference Δn, that is, the sensitivity, is Δd・Ia/M
Therefore, it decreases to 1/M.
また、リニアリテイレンジは、ｄがＭ倍となる
ことからＭ倍大きくなる。 Furthermore, since d is multiplied by M, the linearity range becomes larger by M times.
そして、スリツトの切替えによつても信号処理
系は変更する必要はない。 There is no need to change the signal processing system even when the slit is switched.
（実施例） 第１図は本発明の一実施例を表わす。(Example) FIG. 1 represents one embodiment of the invention.
４は光源、６はレンズ、８はスリツト用円板で
あり、円板８には長さが同じで、スリツト幅がｄ
の高感度分析用スリツト８−１と、スリツト幅が
その10倍の10dの分取用スリツト８−２とが設け
られており、モータ１０の回転により両スリツト
８−１，８−２が切り替えられるようになつてい
る。１２は試料液と対照液とをそれぞれ通液ある
いは収容する２個の容器を有する光学セルであ
り、２個の容器は隔壁１４により分離されてお
り、スリツト８−１又は８−２を通過した光がレ
ンズ１６を経てこの光学セルに入射し、隔壁１６
を透過するときに両容器内の液体の屈折率差Δn
により変位される。１８は反射ミラーで、光学セ
ル１２の透過光を再びその光学セル１２に入射さ
せて変位を増幅させるためのものである。 4 is a light source, 6 is a lens, and 8 is a slit disk.The disk 8 has the same length and a slit width of d.
A slit 8-1 for high-sensitivity analysis and a slit 8-2 for preparative separation with a slit width of 10 d are provided, and both slits 8-1 and 8-2 are switched by the rotation of the motor 10. It's starting to become easier. Reference numeral 12 denotes an optical cell having two containers through which a sample solution and a control solution are passed or stored, respectively. Light enters this optical cell through the lens 16 and the partition wall 16
The refractive index difference Δn of the liquid in both containers when passing through
is displaced by Reference numeral 18 denotes a reflecting mirror for making the transmitted light of the optical cell 12 enter the optical cell 12 again to amplify the displacement.
反射ミラー１８による反射光は再び光学セル１
２、レンズ１６を経て第２図に示されるように光
センサ２上にスリツト８−１又は８−２の像を結
像する。光センサ２上でのスリツト像の光強度
は、スリツト８−１，８−２のいずれの場合でも
一様になるように、光学系が設計されている。 The light reflected by the reflection mirror 18 is returned to the optical cell 1.
2. An image of the slit 8-1 or 8-2 is formed on the optical sensor 2 through the lens 16 as shown in FIG. The optical system is designed so that the light intensity of the slit image on the optical sensor 2 is uniform for both the slits 8-1 and 8-2.
第１図に戻つて、２０，２２はそれぞれ光セン
サのＳ側２−１、Ｒ側２−２の検出信号を電流値
として受け取り電圧値に変換するｉ−Ｖ変換器で
あり、それぞれの出力信号Vs，Vrは前述の(1)，
(2)式に比例する。 Returning to FIG. 1, 20 and 22 are i-V converters that receive the detection signals of the S side 2-1 and R side 2-2 of the optical sensor as current values and convert them into voltage values, and the respective outputs The signals Vs and Vr are as described in (1) above,
It is proportional to equation (2).
２４は両検出信号の和（Vs＋Vr）を算出する
和算素子、２６は差（Vs−Vr）を算出する引算
素子である。２８は光量変動を補正する為の除算
素子であり、和算素子２４と引算素子２６とから
信号を入力して、（Vs−Vr）／（Vs＋Vr）を算
出し、記録計へ信号を送出する。 24 is a summation element that calculates the sum (Vs+Vr) of both detection signals, and 26 is a subtraction element that calculates the difference (Vs-Vr). 28 is a division element for correcting light intensity fluctuations, inputs signals from the summation element 24 and subtraction element 26, calculates (Vs-Vr)/(Vs+Vr), and sends the signal to the recorder. do.
３０はスリツト８−１，８−２の切替えと、光
源４の光量を切り替えるための切替えスイツチで
あり、３２はこの切替えスイツチ３０の出力信号
によりモータ１０を回転させてスリツトを切り替
えるモータ駆動回路、３４はスリツトが切に替え
られたとき、和算素子２４の出力信号（Vs＋
Vr）が一定になるように光源４の光量を制御す
る光源用電源回路であるる。 30 is a changeover switch for switching between the slits 8-1 and 8-2 and the amount of light from the light source 4; 32 is a motor drive circuit that rotates the motor 10 to change over the slits according to the output signal of the changeover switch 30; 34, when the slit is switched, the output signal (Vs+
This is a light source power supply circuit that controls the amount of light from the light source 4 so that Vr) remains constant.
いま、微量分析を行なうために、第１図のよう
に幅の狭い高感度用スリツト８−１が設定されて
いるとする。まず、光学セル１２の両容器内の溶
液の屈折率に差がないとき、光センサ２上のスリ
ツト像が正しく中央にくるように、光学的にゼロ
位置を調整しておく。 Assume now that a narrow high-sensitivity slit 8-1 is set as shown in FIG. 1 in order to perform trace analysis. First, when there is no difference in the refractive index of the solutions in both containers of the optical cell 12, the zero position is optically adjusted so that the slit image on the optical sensor 2 is correctly centered.
次に光学セル１２の両容器に試料液と対照液と
を通液して、その屈折率差がΔnであつたとする
と、光センサ２上の変位Δdは、
Δd＝2l・Δn／ｎ ……(3)
となる。このとき、スリツト８−１の像の幅をd1
とする。 Next, if the sample liquid and the control liquid are passed through both containers of the optical cell 12 and the difference in refractive index is Δn, then the displacement Δd on the optical sensor 2 is Δd=2l・Δn/n... (3) becomes. At this time, the width of the image of slit 8-1 is d 1
shall be.
光センサ２のＳ側２−１、Ｒ側２−２のそれぞ
れの検出信号をＩ−Ｖ変換器２０，２２に入力
し、和算素子２４、引算素子２６を経て、除算素
子２８により出力される信号は、
Δd／d1 ……(4)
に比例したものとなる。 The detection signals of the S side 2-1 and R side 2-2 of the optical sensor 2 are input to the IV converters 20 and 22, passed through the summation element 24 and the subtraction element 26, and are outputted by the division element 28. The resulting signal is proportional to Δd/d 1 ...(4).
次に、切替えイツチ３０によりモータ駆動回路
３２を経てモータ１０を作動させてスリツト用円
板８を180度回転させ、スリツトを分取用の幅の
広い低感度用スリツト８−２に切り替えたとす
る。このとき光センサ２上のスリツト像の幅ｄが
スリツト切替え前の10倍に増大する。光源用電源
回路３４は和算素子２０の出力信号がスリツト切
替え前後で変化しないように光源４の光量を変化
させ、1/10に減少させる。そして、除算素子２８
の出力信号は、Δd／d1と1/10となり、すなわち
感度が1/10により、リニアリテイレンジはスリツ
ト幅に比例して10倍広くなる。 Next, assume that the switching switch 30 operates the motor 10 via the motor drive circuit 32 to rotate the slit disk 8 by 180 degrees, and the slit is switched to the wide low-sensitivity slit 8-2 for preparative separation. . At this time, the width d of the slit image on the optical sensor 2 increases ten times as much as before the slit switching. The light source power supply circuit 34 changes the light amount of the light source 4 so that the output signal of the summation element 20 does not change before and after switching the slit, and reduces it to 1/10. And the division element 28
The output signal of Δd/d is 1/10 , that is, the sensitivity is 1/10, and the linearity range is 10 times wider in proportion to the slit width.
以上の実施例では、スリツトの切替えに伴なう
光源の光量制御を行なうために、和算素子２４の
出力信号（Vs＋Vr）が一定になるように光源用
電源回路３４にフイードバツクをかけているの
で、正確な光量制御が達成されるが、スリツトの
切替えと同時に、スリツト幅に反比例するよう予
め設定された光量に切り替えるようにしてもよ
い。 In the above embodiment, in order to control the light amount of the light source as the slit is switched, feedback is applied to the light source power supply circuit 34 so that the output signal (Vs + Vr) of the summation element 24 is constant. Although accurate light amount control is achieved, the light amount may be switched to a preset light amount that is inversely proportional to the slit width at the same time as the slit is switched.
また、スリツト８−１と８−２の切替え機構と
しては、上記実施例のようにスリツト用円板８を
回転させて行なうものの他、例えば、スライド方
式により切り替えるなど、種々の機構を採用する
ことができる。 In addition to the mechanism for switching between the slits 8-1 and 8-2 by rotating the slit disc 8 as in the above embodiment, various mechanisms may be used, such as switching by a sliding method. I can do it.
そして、スリツトと光源光量の切替えを切替え
スイツチの１個のボタン操作のみで全て自動的に
行なわれるようにしておけば便利である。 It would be convenient if the switching between the slit and the amount of light from the light source could be done automatically by operating only one button on the changeover switch.
(ハ) 発明の効果
本発明の示差屈折計によれば、１台の装置で微
量分析用の高感度示差屈折計と、分取用の低感度
示差屈折計との両用途に使用することができ、し
かもその切替え操作は極めて簡単である。(C) Effects of the Invention According to the differential refractometer of the present invention, one device can be used for both a high-sensitivity differential refractometer for trace analysis and a low-sensitivity differential refractometer for preparative separation. Moreover, the switching operation is extremely simple.
第１図は本発明の一実施例を示す概略図、第２
図は光センサでの検出方法を示す図である。
２……光センサ、４……光源、８−１，８−２
……スリツト、１２……光学セル、３０……切替
えスイツチ、３２……モータ駆動回路、３４……
光源用電源回路。
FIG. 1 is a schematic diagram showing one embodiment of the present invention, and FIG.
The figure is a diagram showing a detection method using an optical sensor. 2... Optical sensor, 4... Light source, 8-1, 8-2
... Slit, 12 ... Optical cell, 30 ... Changeover switch, 32 ... Motor drive circuit, 34 ...
Power supply circuit for light source.
Claims (1)
た２個の容器を有する光学セルに光を入射し、両
容器内の液体の屈折率差に対応した透過光の変位
を測定する示差屈折計において、 スリツト幅の異なる２種類のスリツトと、 光学セルへ入射される光の光源の光量を制御す
る手段と、を備え、 スリツトの切替えと同時に光源の光量をスリツ
ト幅に反比例するように変化させることを特徴と
する示差屈折計。[Claims] 1. Light is incident on an optical cell having two containers separated by a partition wall that is inclined with respect to the direction of light incidence, and the displacement of the transmitted light corresponds to the difference in refractive index of the liquid in both containers. A differential refractometer for measuring slits includes two types of slits with different slit widths and a means for controlling the amount of light from the light source that enters the optical cell, and simultaneously changes the amount of light from the light source to the slit width when switching the slits. A differential refractometer characterized by a change in inverse proportion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10698484A JPS60250230A (en) | 1984-05-26 | 1984-05-26 | Differential refractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10698484A JPS60250230A (en) | 1984-05-26 | 1984-05-26 | Differential refractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60250230A JPS60250230A (en) | 1985-12-10 |
| JPH047828B2 true JPH047828B2 (en) | 1992-02-13 |
Family
ID=14447524
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10698484A Granted JPS60250230A (en) | 1984-05-26 | 1984-05-26 | Differential refractometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60250230A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2504356B2 (en) * | 1992-04-09 | 1996-06-05 | 株式会社島津製作所 | Differential refractometer |
| JP4577177B2 (en) * | 2005-09-30 | 2010-11-10 | 株式会社島津製作所 | Differential refractive index detector and adjustment method thereof |
| ES2887026B2 (en) * | 2020-06-18 | 2023-12-22 | Univ Cantabria | REFRACTOMETER AND METHOD OF MEASURING THE REFRACTION INDEX OF A SUBSTANCE |
-
1984
- 1984-05-26 JP JP10698484A patent/JPS60250230A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60250230A (en) | 1985-12-10 |
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| LAPS | Cancellation because of no payment of annual fees |