JPH0638069B2 - Differential refractometer - Google Patents
Differential refractometerInfo
- Publication number
- JPH0638069B2 JPH0638069B2 JP60067460A JP6746085A JPH0638069B2 JP H0638069 B2 JPH0638069 B2 JP H0638069B2 JP 60067460 A JP60067460 A JP 60067460A JP 6746085 A JP6746085 A JP 6746085A JP H0638069 B2 JPH0638069 B2 JP H0638069B2
- Authority
- JP
- Japan
- Prior art keywords
- light
- light receiving
- receiving element
- pair
- monitor
- 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
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】 産業上の利用分野 本発明は、液体クロマトグラフに用いられる示差屈折計
に関する。TECHNICAL FIELD The present invention relates to a differential refractometer used in a liquid chromatograph.
従来の技術 液体クロマトグラフに用いられる示差屈折計において、
フローセルや光学素子等の汚れによる測定誤差を除くた
めの補正技術として、例えば実開昭４８−４５６９１号
公報には、フローセルにおいて屈折された光を一対の受
光素子により受光し、その受光器出力の加算出力と減算
出力とを除算器により除算する手法が開示され、また特
開昭５９−１２５０４１号公報には、フローセルにおい
て屈折された光を一対の受光素子により受光し、その受
光器出力を加算し、その加算電圧に基づいて一対の受光
素子に受光される総光量が一定となるように発光素子の
発光量を制御する手法が開示されている。Conventional technology In the differential refractometer used for liquid chromatograph,
As a correction technique for eliminating a measurement error due to contamination of a flow cell, an optical element, etc., for example, Japanese Utility Model Laid-Open No. 48-45691 discloses that light refracted in a flow cell is received by a pair of light receiving elements and the output of the light receiver is A method of dividing an addition output and a subtraction output by a divider is disclosed, and Japanese Patent Laid-Open No. 59-125041 discloses that light refracted in a flow cell is received by a pair of light receiving elements, and the outputs of the light receiving elements are added. However, there is disclosed a method of controlling the light emission amount of the light emitting element so that the total light amount received by the pair of light receiving elements becomes constant based on the added voltage.
発明が解決しようとする問題点 しかしながら、前記した従来技術の前者によると、除算
器自体は高価であり、かつノイズが多く、その上ダイナ
ミツクレンジが狭いという欠点があり、また従来技術の
後者の場合は一般に一対の受光素子や一対の増幅器等に
由来する感度差が存在し、この一対の感度差を除かない
限り正確な光量変化による測定誤差の補正をすることが
できない。そこで、前記した一対の感度差の補正を行な
う必要があるが、一対の感度差の補正のための調整作業
に手間がかかるという欠点がある。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention However, according to the former of the above-mentioned prior art, the divider itself is expensive, has a lot of noise, and has a drawback that the dynamic range is narrow, and the latter of the conventional art has the drawback. In this case, generally, there is a difference in sensitivity due to a pair of light receiving elements, a pair of amplifiers, etc., and it is impossible to correct the measurement error due to an accurate change in the light amount unless the pair of sensitivity differences are removed. Therefore, it is necessary to correct the pair of sensitivity differences as described above, but there is a drawback that the adjustment work for correcting the pair of sensitivity differences takes time.
そこで、本発明は、前記した従来技術の有する問題点に
かんがみ、高価な除算器を必要とすることなく、かつ受
光素子の検出感度を補正するための調整作業を必要とせ
ずに、フローセルや光学素子等の汚れによる受光素子の
光量の変動を正確に補正する示差屈折計を提供すること
を目的とする。Therefore, in view of the above-mentioned problems of the conventional technology, the present invention does not require an expensive divider, and does not require an adjustment work for correcting the detection sensitivity of the light receiving element, and thus the flow cell and the optical system. An object of the present invention is to provide a differential refractometer that accurately corrects fluctuations in the light amount of a light receiving element due to dirt on the element and the like.
問題点を解決するための手段 本発明は、前記目的を達成するため、試料液と標準液と
が通流するフローセルと、前記フローセルに送光する発
光素子と、前記発光素子を付勢する光源用電源と、前記
フローセルにおいて屈折された光を受光する示差出力検
出用の一対の受光素子とを具備するものにおいて、前記
示差出力検出用の一対の受光素子と一体に形成された単
一のモニタ用受光素子と、前記モニタ用受光素子の出力
が入力され、該モニタ用受光素子に受光される光量が一
定となるように前記発光素子の発光量を制御すべく、前
記光源用電源を制御する制御手段とを備える示差屈折計
にある。Means for Solving the Problems In order to achieve the above object, the present invention provides a flow cell through which a sample solution and a standard solution flow, a light emitting element for sending light to the flow cell, and a light source for energizing the light emitting element. A power source and a pair of light receiving elements for detecting a differential output for receiving light refracted in the flow cell, wherein a single monitor integrally formed with the pair of light receiving elements for detecting the differential output The light-source power source is controlled so that the output of the light-receiving element for monitoring and the output of the light-receiving element for monitoring are input and the light-emitting amount of the light-emitting element is controlled so that the amount of light received by the light-receiving element for monitoring becomes constant. And a differential refractometer with control means.
作用 発光素子の発光光をフローセルに送光し、試料液により
屈折されたフローセルからの光をモニタ用受光素子にて
受光し、その受光出力を制御手段に加え、モニタ用受光
素子に受光される光量が常に一定となるように発光素子
の発光量を制御すべく、光源用電源を制御する。Function Light emitted from the light emitting element is sent to the flow cell, light from the flow cell refracted by the sample liquid is received by the monitor light receiving element, and the received light output is applied to the control means and received by the monitor light receiving element. The power source for the light source is controlled to control the light emission amount of the light emitting element so that the light amount is always constant.
実施例 以下に、本発明の示差屈折計の実施例を説明する。Examples Examples of the differential refractometer of the present invention will be described below.
図はいずれも本発明の実施例を示すもので、第１図にお
いて、１は光源用電源、２は発光素子であり、３はレン
ズ、４は示差出力検出用の一対のスリツトとモニタ用ス
リツトとが穿設されたスリツト板であり、５はレンズ、
６は同様に示差出力検出用の一対のスリツトとモニタ用
スリツトとが穿設されたスリツト板である。７はフロー
セルで、標準液と試料液とがそれぞれ通流する標準セル
７ａと試料セル７ｂとからなり、８はフローセル７から
の入射光を反射するための鏡である。９は受光素子で、
第２図に示すように基板の左右に示差出力検出用の一対
の受光素子９ａおよび９ｂと、これらの上部に一体に形
成された単一のモニタ用受光素子９ｃとが配設されてい
る。１０は示差信号出力回路で、示差出力検出用の一対
の受光素子９ａおよび９ｂの出力電流を電圧に変換する
周知の電流電圧変換器と減算器が設けられている。１１
は制御手段としての制御回路であり、その具体的構成を
第３図に基づいて説明すると、１２は電流電圧変換器で
あり、モニタ用受光素子９ｃからの出力電流ＩMを電圧
ＶMに変換する。１３は抵抗Ｒと、コンデンサＣと、オ
ペアンプとからなる積分器であり、オペアンプの反転側
入力端子には電圧ＶMが、その非反転側入力端子には電
圧ＶRが加えられた分圧用抵抗１４からの分圧された基
準電圧Ｖrが入力されている。１５は制御用トランジス
タで、積分器１３の出力電圧をそのベースに入力され、
光源用電源Ｖcから送流される電流を制御し、発光素子
２の発光量を制御する。Each of the figures shows an embodiment of the present invention. In FIG. 1, 1 is a light source power source, 2 is a light emitting element, 3 is a lens, 4 is a pair of slits for differential output detection and a monitor slit. Is a slit plate with holes, 5 is a lens,
Similarly, 6 is a slit plate in which a pair of slits for differential output detection and a monitor slit are provided. Reference numeral 7 is a flow cell, which is composed of a standard cell 7a and a sample cell 7b through which a standard solution and a sample solution respectively flow, and 8 is a mirror for reflecting incident light from the flow cell 7. 9 is a light receiving element,
As shown in FIG. 2, a pair of light receiving elements 9a and 9b for detecting a differential output, and a single monitor light receiving element 9c integrally formed on the upper side of the light receiving elements 9a and 9b are disposed on the left and right sides of the substrate. Reference numeral 10 is a differential signal output circuit, which is provided with a known current-voltage converter and a subtracter for converting the output currents of the pair of light receiving elements 9a and 9b for detecting the differential output into voltage. 11
Is a control circuit as a control means, and its specific configuration will be described with reference to FIG. 3. Reference numeral 12 is a current-voltage converter, which converts an output current I M from the monitor light-receiving element 9c into a voltage V M. To do. 13 a resistor R, a capacitor C, and an integrator composed of an operational amplifier, the inverting input terminal of the operational amplifier is the voltage V M, the non-inverting side input dividing resistor the voltage V R applied to the terminal The divided reference voltage V r from 14 is input. 15 is a control transistor, the output voltage of the integrator 13 is input to its base,
The amount of light emitted from the light emitting element 2 is controlled by controlling the current sent from the light source power source V c .
次に、本実施例装置の作用を説明すると、光源用電源１
により付勢された発光素子２からの発光光はレンズ３と
スリツト板４とにより平行光束とされ、かつスリツト板
４により示差出力検出用の一対の光束とモニタ用光束と
なつてレンズ５とスリツト板６を介してフローセル７を
通過し、鏡８により反射され、再びフローセル７と、ス
リツト板６とレンズ５とを介し、受光素子９に向けて送
光される。その際、試料セル７ｂを通流する試料液によ
り示差出力検出用の一対の光束とモニタ用光束とが屈折
され、一対の受光素子９ａおよび9bに、そしてモニタ用
受光素子９ｃにそれぞれ受光される。一対の受光素子９
ａと９ｂに受光された光束は電流に変換され、示差信号
出力回路１０に入力され、ここで電流電圧変換器により
それぞれ電圧に変換され、これらの電圧を減算器により
減算し、示差信号として不図示のデータ処理装置に入力
する。一方、モニタ用受光素子９ｃに受光された光束は
電流ＩMとなつて電流電圧変換器１２に入力され、その
出力電圧ＶMを積分器１３に入力する。電圧ＶMが基準電
圧Ｖrより高くなると、抵抗ＲからコンデンサＣに充電
電流が流れ、積分器13の出力電圧が低下し、これにより
トランジスタ15のベース電流が減少する。従つて、光源
用電源電圧Ｖcから発光素子２に送流されるエミツタ電
流が減少し、発光素子２の光量が減少する。この光量の
減少がモニタ用受光素子９ｃにより検出され、その出力
電流が減少する。そして、モニタ用受光素子９ｃの出力
電圧が基準電圧Ｖrより減少すると、前記した場合と逆
の制御を行なう。このようにして、モニタ用受光素子９
ｃからの出力電圧が基準電圧Ｖrと常に等しく制御さ
れ、モニタ用受光素子９ｃに受光される光量が一定とな
り、従つて示差出力検出用受光素子９ａと９ｂに受光さ
れる光量が常に一定となる。Next, the operation of the apparatus of this embodiment will be described. The light source power source 1
The light emitted from the light emitting element 2 which is urged by the lens 3 and the slit plate 4 are collimated into a parallel luminous flux, and the slit plate 4 forms a pair of luminous flux for detecting a differential output and a monitoring luminous flux to form the lens 5 and the slit. The light passes through the flow cell 7 through the plate 6, is reflected by the mirror 8, and is again transmitted toward the light receiving element 9 through the flow cell 7, the slit plate 6 and the lens 5. At this time, the pair of light beams for differential output detection and the monitor light beam are refracted by the sample liquid flowing through the sample cell 7b, and are received by the pair of light receiving elements 9a and 9b and the monitor light receiving element 9c, respectively. . A pair of light receiving elements 9
The light fluxes received by a and 9b are converted into currents and input to the differential signal output circuit 10, where they are converted into respective voltages by the current-voltage converters, and these voltages are subtracted by the subtractors to obtain the differential signals. Input to the illustrated data processing device. On the other hand, the luminous flux received by the monitor light-receiving element 9c is input to the current-voltage converter 12 as a current I M, and its output voltage V M is input to the integrator 13. When the voltage V M becomes higher than the reference voltage V r , a charging current flows from the resistor R to the capacitor C and the output voltage of the integrator 13 decreases, which decreases the base current of the transistor 15. Therefore, the emitter current sent from the light source power source voltage V c to the light emitting element 2 decreases, and the light amount of the light emitting element 2 decreases. This decrease in the amount of light is detected by the monitor light receiving element 9c, and the output current thereof is decreased. When the output voltage of the monitor light receiving element 9c decreases below the reference voltage V r , the control reverse to the above case is performed. In this way, the monitor light receiving element 9
The output voltage from c is always controlled to be equal to the reference voltage V r, and the amount of light received by the monitor light receiving element 9c becomes constant, and thus the amount of light received by the differential output detection light receiving elements 9a and 9b is always constant. Become.
発明の効果 以上説明したように本発明によると、単一のモニタ用受
光素子を設け、このモニタ用受光素子の出力を制御手段
に加え、モニタ用受光素子に受光される光量が常に一定
となるように光源用電源を制御し、発光素子の発光量を
制御する構成であるから、従来装置のように高価な除算
器を必要とする補正手段を採用することがなく、またモ
ニタ用受光素子が単一構成であるから、その検出感度の
差異を問題とすることがなく、従つてモニタおよび示差
出力検出兼用の一対の受光素子や増幅器を用いる従来装
置のように、それぞれの受光素子の感度差や抵抗のばら
つきによる感度差を補正するための調整作業を必要とせ
ずに、フローセルや光学素子の汚れ等によるモニタ用受
光素子に受光される光量の変動を簡単にかつ正確に補正
することができる。As described above, according to the present invention, a single monitor light-receiving element is provided, the output of this monitor light-receiving element is added to the control means, and the amount of light received by the monitor light-receiving element is always constant. As described above, since the power source for the light source is controlled to control the light emission amount of the light emitting element, it is not necessary to employ a correction unit that requires an expensive divider unlike the conventional device, and the monitor light receiving element is Since it has a single configuration, the difference in detection sensitivity does not pose a problem, and therefore the difference in sensitivity between the light receiving elements is different, as in conventional devices that use a pair of light receiving elements and amplifiers for both monitor and differential output detection. It is possible to easily and accurately correct fluctuations in the amount of light received by the monitor light-receiving element due to contamination of the flow cell or optical elements, without the need for adjustment work to correct the sensitivity difference due to variations in resistance and resistance. You can
【図面の簡単な説明】 第１図は本発明の示差屈折計の実施例の構成図、第２図
は第１図に用いられる受光素子の上面図、第３図は第１
図に用いられる制御回路の回路図である。 １は光源用電源、２は発光素子、９は受光素子、９ａと
９ｂは示差出力検出用の一対の受光素子、９ｃはモニタ
用受光素子、１１は制御回路を示す。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a configuration diagram of an embodiment of a differential refractometer of the present invention, FIG. 2 is a top view of a light receiving element used in FIG. 1, and FIG.
It is a circuit diagram of a control circuit used in the figure. Reference numeral 1 is a light source power source, 2 is a light emitting element, 9 is a light receiving element, 9a and 9b are a pair of light receiving elements for differential output detection, 9c is a monitor light receiving element, and 11 is a control circuit.
Claims (1)
と、前記フローセルに送光する発光素子と、前記発光素
子を付勢する光源用電源と、前記フローセルにおいて屈
折された光を受光する示差出力検出用の一対の受光素子
とを具備するものにおいて、 前記示差出力検出用の一対の受光素子と一体に形成され
た単一のモニタ用受光素子と、該モニタ用受光素子の出
力が入力され、該モニタ用受光素子に受光される光量が
一定となるように前記発光素子の発光量を制御すべく、
前記光源用電源を制御する制御手段とを備える示差屈折
計。1. A flow cell through which a sample solution and a standard solution flow, a light emitting element for sending light to the flow cell, a light source power source for energizing the light emitting element, and a light refracted in the flow cell. In one comprising a pair of light receiving elements for differential output detection, a single monitor light receiving element formed integrally with the pair of light receiving elements for differential output detection, and the output of the monitor light receiving element is input. In order to control the light emission amount of the light emitting element so that the light amount received by the monitor light receiving element becomes constant,
A differential refractometer comprising: a control unit that controls the power source for the light source.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60067460A JPH0638069B2 (en) | 1985-03-30 | 1985-03-30 | Differential refractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60067460A JPH0638069B2 (en) | 1985-03-30 | 1985-03-30 | Differential refractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61226640A JPS61226640A (en) | 1986-10-08 |
| JPH0638069B2 true JPH0638069B2 (en) | 1994-05-18 |
Family
ID=13345579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60067460A Expired - Fee Related JPH0638069B2 (en) | 1985-03-30 | 1985-03-30 | Differential refractometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0638069B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03162651A (en) * | 1989-11-20 | 1991-07-12 | Shimadzu Corp | Polarization type differential refractometer |
| JP2732320B2 (en) * | 1990-10-31 | 1998-03-30 | 有限会社島村計器製作所 | Differential refractive index detector for liquid chromatography |
| 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 |
| JP5309785B2 (en) * | 2008-08-21 | 2013-10-09 | 東ソー株式会社 | Differential refractometer |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5147354B2 (en) * | 1971-12-29 | 1976-12-14 | ||
| JPS5935801U (en) * | 1982-08-31 | 1984-03-06 | 日野自動車株式会社 | Measuring instrument |
| JPS59125041A (en) * | 1982-12-29 | 1984-07-19 | Showa Denko Kk | Polarization type differential refractometer |
-
1985
- 1985-03-30 JP JP60067460A patent/JPH0638069B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61226640A (en) | 1986-10-08 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |