JPS60209167A - Method and device for capturing and detecting electron - Google Patents
Method and device for capturing and detecting electronInfo
- Publication number
- JPS60209167A JPS60209167A JP6470384A JP6470384A JPS60209167A JP S60209167 A JPS60209167 A JP S60209167A JP 6470384 A JP6470384 A JP 6470384A JP 6470384 A JP6470384 A JP 6470384A JP S60209167 A JPS60209167 A JP S60209167A
- Authority
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- Japan
- Prior art keywords
- gas
- radiation source
- electrons
- electron capture
- purging gas
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
- G01N27/66—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber and measuring current or voltage
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Toxicology (AREA)
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- General Physics & Mathematics (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Description
【発明の詳細な説明】
(イ)ff、楽土の利用分野
本発明は、電子捕獲検出方法及びその装置に関し、特に
、〃スクロマトグラフ分析装置の検出器として適する電
子捕獲検出方法及びその装置に関する。電子捕獲検出器
は、ハロゲン、硫黄化合物、多核芳香族炭化水素等電子
親和力の強い化合物に高い応答力を示し、農薬、その他
環境汚染物質の微量分析等に広く利用されている。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Application of ff, Rakudo The present invention relates to an electron capture detection method and device thereof, and more particularly to an electron capture detection method and device suitable as a detector for a chromatographic analyzer. Electron capture detectors exhibit high responsiveness to compounds with strong electron affinity, such as halogens, sulfur compounds, and polynuclear aromatic hydrocarbons, and are widely used for trace analysis of agricultural chemicals and other environmental pollutants.
(ロ)従来技術
ハロゲン、酸素及びイ、オウ等の化合物並びに多核芳香
族炭化水素などの電子親和力の強い化合物を分析するの
に、窒素キャリヤーがス中にこの種化合物を含む試料ガ
スに放射線を照射して、キャリヤーガスの窒素をイオン
化させ、このM離電子をキャリヤーガス中に含有される
電子親和力の強い化合物に捕獲させ、その電離電流をめ
て行うのは、例えば、電子捕獲検出器として既に公知で
ある。(b) Prior art In order to analyze compounds with strong electron affinity such as halogens, oxygen, and compounds such as sulfur and sulfur, as well as polynuclear aromatic hydrocarbons, a nitrogen carrier is used to irradiate a sample gas containing such compounds with radiation. For example, an electron capture detector uses irradiation to ionize nitrogen in a carrier gas, captures the M electrons in a compound with strong electron affinity contained in the carrier gas, and collects the ionization current. It is already publicly known.
ところで、従来の電子捕獲検出器では、キヤ々ツヤーガ
スの窒素をイオン化する関係上試料ガスに直接放射線を
照射しており、そのために、放射性同位体線源(以下放
射線源という。)は、カラム流出ガスに直接触れる箇所
に設けられて(する。しかし、このように放射線源を試
料ガスに直接触れる箇所に設けてお(と、長時間使用す
る間に放射線源が汚れ、放射線の照射が一様でなくなり
、感度の低下をきたす原因でもあった。By the way, in conventional electron capture detectors, the sample gas is directly irradiated with radiation in order to ionize the nitrogen in the carbon gas. However, if the radiation source is installed in a place where it comes into direct contact with the sample gas, the radiation source will become dirty during long-term use and the radiation will not be irradiated uniformly. This was also the cause of a decrease in sensitivity.
一方、放射線源として使用される質量数63のニッケル
板は、3011X40Hの大きさのものであり、これを
円筒状に形成して放射線源とするために、電子捕獲室は
ほぼ10111!径の円筒の大きさになり、キャピラリ
ーカラムを使用する場合には、デッドボリュムが太き(
なり問題であった。On the other hand, the nickel plate with a mass number of 63 used as a radiation source has a size of 3011 x 40H, and in order to form it into a cylindrical shape and use it as a radiation source, the electron capture chamber is approximately 10111 mm! When using a capillary column, the dead volume is thick (
That was a problem.
といって、周囲を狭めると、放射線が窒素に当らずに電
子捕獲室壁に当る率が多くなり、イオン化の効率すなわ
ち、感度が低下するので好ましいこととはいえない。However, if the circumference is made narrower, the ratio of radiation hitting the electron trapping chamber wall instead of hitting nitrogen increases, which lowers the ionization efficiency, that is, the sensitivity, which is not desirable.
(ハ) 目的
本発明は、従来の電子捕獲検出法及び電子捕獲検出器に
おける問題点を解消するものであり、キャピラリーカラ
ムクロマトグラフの検出器として使用して、デッドボリ
ュムを生じないで、しかも、高感度で検出できる電子捕
獲検出法及び電子捕獲検出器を提供するものである。(c) Purpose The present invention solves the problems in conventional electron capture detection methods and electron capture detectors, and can be used as a detector for capillary column chromatography without producing dead volume and with high performance. The present invention provides an electron capture detection method and an electron capture detector that can detect with high sensitivity.
(ニ)構成
本発明は、パージガス流を、α線またはβ線放射線源上
に流して、該パージガスをイオン化させ、このイオン化
したパージガス流を、試料ガス流と混合させて、この混
合ガス流の電離電流を測定することを特徴とするガス中
の電子親和力の強い化合物の分析方法及び、電子捕獲反
応室内側に設けられたα線またはβ線を放射する放射線
源と、該放射線源の位置よりも分離室側に近い位置で室
内にn+1口するパージガス導入口と、該放射線源より
も出口側に近い位置で室内に開口する試料ガス導入ノズ
ルを具備することを特徴とする電子捕獲検出器にある。(D) Structure The present invention allows a purge gas flow to flow over an alpha or beta radiation source to ionize the purge gas, and mixes the ionized purge gas flow with a sample gas flow to form the mixed gas flow. A method for analyzing compounds with strong electron affinity in a gas characterized by measuring ionization current, a radiation source that emits α-rays or β-rays provided inside an electron capture reaction chamber, and a position of the radiation source An electron capture detector characterized in that it is equipped with a purge gas introduction port that opens into the chamber at a position closer to the separation chamber side, and a sample gas introduction nozzle that opens into the chamber at a position closer to the exit side than the radiation source. be.
本発明において、パージガス流は、放射線源上を流れて
、放射線源の表面を常に清浄に保つと共にイオン化され
て、電子捕獲反応の電子を供給するものである。パージ
ガスとしては、イオン化され易いガス、例えば、窒素及
び希ガス等が使用される。アルゴンを使用する場合は、
イオン化と共に準安定アルゴン原子が生成して、試料分
子を陽イオンにイオン化するので、これを防止するため
に、メタンが10%程度加えられる。パージガスは、キ
ャリヤーガスと同一のものをfSII用するのがキャリ
ヤーガス源を使用できるので好ましいが、必ずしも同一
にする必要はない。In the present invention, the purge gas stream flows over the radiation source to keep the surface of the radiation source clean and is ionized to provide electrons for the electron capture reaction. As the purge gas, gases that are easily ionized, such as nitrogen and rare gases, are used. If using argon,
Metastable argon atoms are generated with ionization and ionize sample molecules into positive ions, so to prevent this, approximately 10% methane is added. It is preferable to use the same purge gas as the carrier gas for fSII since the carrier gas source can be used, but it is not necessary to use the same purge gas.
本発明において、パージガス流のイオン化流路は試料ガ
ス流路と区別されていれば如何なる形式のものとするこ
ともできる。イオン化されたパージガス流と試料ガス流
の混合は、電子捕獲反応が速やかに行えるように混合す
れば足り、例えば同方向に流して混合するなど種々の混
合方法を採用することができる。In the present invention, the ionization channel for the purge gas flow can be of any type as long as it is distinct from the sample gas channel. It is sufficient to mix the ionized purge gas flow and the sample gas flow so that the electron capture reaction can be performed quickly, and various mixing methods can be employed, such as mixing them by flowing them in the same direction.
放射線源としては、63N i線源が一般に使用される
が、コノ外に、”HN 85Kr、 ”S rs ”’
T es目’ P ml 226Rfl、 ” ’ A
mが使用される。これらの中で85Kr190Srに
ついては、β線のエネルギーが強いために副次的に発生
する制動X線に注意を要する。また、3Hは気体である
ために、5cHn、TiHn等の形で使用されるが、T
iHnは、225℃以上の高温では、3Hの流出が多く
なるために高温での使用には注意を要する。As a radiation source, a 63N i-ray source is generally used, but in addition to this, "HN 85Kr", "Srs"'
T es' P ml 226Rfl, ” 'A
m is used. Among these, for 85Kr190Sr, attention must be paid to the secondary generation of bremsstrahlung X-rays due to the strong beta-ray energy. In addition, since 3H is a gas, it is used in the form of 5cHn, TiHn, etc., but T
iHn must be used with caution at high temperatures, since 3H flows out in large quantities at high temperatures of 225° C. or higher.
本発明の電子捕獲検出法を実施する一例として、電子捕
獲検出器のセルを二重円筒構造に形成したものを使用す
ることができる。この場合、放射線源は内側及び外側の
何れに配置してもよい。内側円筒管内にキャピラリーカ
ラム又はカラムを挿通して、試料ノズルに接続させるよ
うにしてもよく、また、直接、試料ノズルを内側円筒の
代りに電子itl獲反応室内に延長させて配置してもよ
い。試料ノズルは、流出する試料ガスが放射線源に直接
触れないように、放射線源よりも出口に近い位置に設け
られる。ノズルから流出した試料ガスは、周囲から流入
するパージガスと直ちに混合して、電子捕獲反応が行わ
れる。パージガス導入口は、放射線源よりも出口から離
れた位置に設けられる。As an example of carrying out the electron capture detection method of the present invention, it is possible to use an electron capture detector having cells formed in a double cylindrical structure. In this case, the radiation source may be placed either inside or outside. A capillary column or column may be inserted into the inner cylindrical tube and connected to the sample nozzle, or the sample nozzle may be directly extended into the electron capture reaction chamber instead of the inner cylinder. The sample nozzle is provided at a position closer to the exit than the radiation source so that the outflowing sample gas does not come into direct contact with the radiation source. The sample gas flowing out from the nozzle immediately mixes with the purge gas flowing in from the surroundings, and an electron capture reaction takes place. The purge gas inlet is provided at a position farther from the outlet than the radiation source.
このようにすることによって、放射線源はパージガス流
路に配置されることになり、そして、パージガスが放射
線源の表面上を流れてイオン化されると共に放射線源の
表面を常に清浄に保つことができ、また、試料ガスが外
側流路内に侵入するのを防止することができる。By doing so, the radiation source is placed in the purge gas flow path, and the purge gas flows over the surface of the radiation source to be ionized and to keep the surface of the radiation source clean at all times. Further, it is possible to prevent the sample gas from entering the outer flow path.
(ホ)実施例
図は、本発明の一実施例の電子捕獲検出器におけるセル
部分の概略の断面図である。以下、この図を参照して、
本発明の具体化の例を詳細に説明するが、本発明は、こ
の説明によって何ら限定されるものではない。(e) Example diagram is a schematic cross-sectional view of a cell portion in an electron capture detector according to an example of the present invention. Referring to this figure below,
Although examples of embodiments of the present invention will be described in detail, the present invention is not limited to this explanation in any way.
本発明の電子捕獲検出器のセル全体が1で示されている
。セル1は、ステンレス製のケーシング2で形成され、
ケーシング2の上端は窄まって細いガス流出路3を形成
する。このガス流出路3の上端には、絶縁体4が気密に
設けられ、この絶縁体4を挿通し、ガス流出路3を通っ
て、コレクタ電極5が配設されている。このガス流出路
3の上方側壁部には排気口6が形成されている。他方、
ケーシング2の下端には、絶縁性の気密部材7を介して
ステンレス製のノズル8が挿通保持されており、このノ
ズル8の下端には、分離カラム9が0−リング10を介
して袋ナツト11により気密に取り伺けられている。The entire cell of the electron capture detector of the present invention is indicated at 1. The cell 1 is formed of a stainless steel casing 2,
The upper end of the casing 2 is narrowed to form a narrow gas outlet passage 3. An insulator 4 is airtightly provided at the upper end of the gas outlet passage 3, and a collector electrode 5 is provided through the insulator 4 and through the gas outlet passage 3. An exhaust port 6 is formed in the upper side wall of the gas outlet passage 3. On the other hand,
A stainless steel nozzle 8 is inserted into the lower end of the casing 2 through an insulating airtight member 7, and a separation column 9 is connected to a cap nut 11 through an O-ring 10 at the lower end of the nozzle 8. The investigation is being conducted in an airtight manner.
ケーシング2の側壁部には例えば、”Niのような放射
線源12が設けられ、その下方側壁部にパージガス導入
口13が設けられる。ノス゛ル8の開口端部14は、ノ
ズル8がら流出する試料ガスが、放射線源12が配設さ
れるパージガス流路に侵入しないようにガス流出路3の
入口に近づけて設けられる。このようにすることによっ
て、デッドボリウムを少くすることができる。A radiation source 12 made of, for example, Ni is provided on the side wall of the casing 2, and a purge gas inlet 13 is provided on the lower side wall. is provided close to the entrance of the gas outlet path 3 so as not to invade the purge gas flow path in which the radiation source 12 is disposed.By doing so, the dead volume can be reduced.
本発明の電子捕獲検出器は、パージガスがパージガス導
入口13からセル内に導入され、ケーシング2とノズル
8に囲まれた空間15を流れる。In the electron capture detector of the present invention, purge gas is introduced into the cell from the purge gas inlet 13 and flows through a space 15 surrounded by the casing 2 and the nozzle 8 .
パージガスは、この空間を流れる開に、放射線源12か
ら放射されるβ線によってイオン化され、電子を生成す
る。この電子を生成したパージガス流は、ガス流出路3
の入口に向って流れ、ノズル8の開口端部14を流出す
る試料ガスと該開口端部14の上方の空間で混合し、試
料ガス中の親電子化合物は、パージがス中の電子を捕獲
して、コレクタ電極5に流れる電離電流を減少させる。As the purge gas flows through this space, it is ionized by the beta rays emitted from the radiation source 12 and generates electrons. The purge gas flow that generated these electrons is transferred to the gas outlet path 3.
The electrophilic compound in the sample gas flows toward the inlet of the nozzle 8 and mixes with the sample gas flowing out of the open end 14 of the nozzle 8 in the space above the open end 14, and the electrophilic compound in the sample gas captures electrons in the gas. As a result, the ionization current flowing through the collector electrode 5 is reduced.
このコレクタ電極5に流れる電離電流を測定して、その
値から親電子化合物濃度をめる。The ionization current flowing through the collector electrode 5 is measured, and the electrophilic compound concentration is calculated from the measured value.
本発明の電子捕獲検出器においては、放射線源12の表
面上は繰返して使用したにも拘らず清浄であった。また
、キャピラリーカラムを使用しても、ピークの拡がりが
みられなかった。In the electron capture detector of the present invention, the surface of the radiation source 12 remained clean despite repeated use. Furthermore, no peak broadening was observed even when a capillary column was used.
(へ)効果
本発明は、パージガスをイオン化ガスとして使用するの
で、放射線照射によるイオン化工程と電子捕獲反応工程
とを分離することができる。したがって、試料ガスが放
射線源に直接触れることがなくなり、放射線源の試料ガ
スによる馬乗を避けることができる。したがって、放射
線源の清掃及びそれによる稼動体止時間が減少するので
、分析コストを低下することができる。(f) Effects In the present invention, since the purge gas is used as the ionization gas, the ionization process by radiation irradiation and the electron capture reaction process can be separated. Therefore, the sample gas does not come into direct contact with the radiation source, and riding of the radiation source by the sample gas can be avoided. Therefore, the cleaning of the radiation source and the resulting downtime of the moving body are reduced, so that analysis costs can be reduced.
しかも、本発明は、イオン化工程と電子捕獲室を分離で
きるので従来の電子捕獲検出器のように、イオン化工程
と電子捕獲反応工程を同時に行なわなくて済むために、
放射線照射効率を−yf′慮することなく電子捕獲反応
のみの反応室を形成することができるから、電子捕獲反
応室の大きさは、従来の電子捕獲検出器の場合と比較し
て、者しく減少することができるので、キャピラリーカ
ラムを使用しても、ピークの拡がりを防ぐことができる
。Moreover, the present invention allows the ionization process and the electron capture chamber to be separated, so unlike conventional electron capture detectors, the ionization process and electron capture reaction process do not have to be performed at the same time.
Since it is possible to form a reaction chamber for only electron capture reactions without considering radiation irradiation efficiency -yf', the size of the electron capture reaction chamber can be reduced compared to the case of conventional electron capture detectors. Therefore, even if a capillary column is used, peak broadening can be prevented.
図は、本発明の一実施例の電子捕獲検出器におけるセル
部分の概略の断面図である。
図中符号については、1はセル、2はケーシング、3は
ガス流出路、4は絶縁体、5はコレクタ電極、6は排気
口、7は気密部材、8はノズル、9は分離カラム、10
はO−リング、11は袋ナツト、12は放射線源、13
はパージガス導入口及び14はノズル開口である。The figure is a schematic cross-sectional view of a cell portion in an electron capture detector according to an embodiment of the present invention. Regarding the symbols in the figure, 1 is a cell, 2 is a casing, 3 is a gas outlet path, 4 is an insulator, 5 is a collector electrode, 6 is an exhaust port, 7 is an airtight member, 8 is a nozzle, 9 is a separation column, 10
is an O-ring, 11 is a cap nut, 12 is a radiation source, 13
1 is a purge gas inlet and 14 is a nozzle opening.
Claims (1)
上に流して、該パージガスをイオン化させ、このイオン
化したパージガス流を、試料が電流と混合させて、この
混合ガス流の電離電流を測定することを特徴とするガス
中の電子親和力の強い化合物の分析方法。 2、電子捕獲反応室内側に設けられたα線またはβ線を
放射する放射性同位体#i源と、該放射性同位体線源の
位置よりも出口側に遠い位置で室内に開1コするバージ
ガス導入口と、該放射性同位体線源よりも出口側に近い
位置で室内に開口する試料ガス導入ノズルを兵傾1する
ことを特徴とする電子捕獲検出器。[Scope of Claims] 1. A purge gas stream is passed over an alpha or beta radioisotope source to ionize the purge gas, and the sample mixes the ionized purge gas stream with an electric current to cause this mixing. A method for analyzing compounds with strong electron affinity in a gas, which is characterized by measuring the ionization current of a gas flow. 2. A radioisotope #i source that emits α-rays or β-rays installed inside the electron capture reaction chamber, and a barge gas that opens into the chamber at a position farther from the exit side than the position of the radioisotope source. An electron capture detector characterized in that an inlet and a sample gas inlet nozzle that opens into the chamber at a position closer to the outlet than the radioisotope source are arranged side by side.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6470384A JPS60209167A (en) | 1984-03-31 | 1984-03-31 | Method and device for capturing and detecting electron |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6470384A JPS60209167A (en) | 1984-03-31 | 1984-03-31 | Method and device for capturing and detecting electron |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS60209167A true JPS60209167A (en) | 1985-10-21 |
JPH0572540B2 JPH0572540B2 (en) | 1993-10-12 |
Family
ID=13265765
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP6470384A Granted JPS60209167A (en) | 1984-03-31 | 1984-03-31 | Method and device for capturing and detecting electron |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS60209167A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62115657U (en) * | 1986-01-16 | 1987-07-23 | ||
WO2009109688A1 (en) * | 2008-03-04 | 2009-09-11 | Pegasor Oy | Particle measurement process and apparatus |
WO2012089924A1 (en) * | 2010-12-31 | 2012-07-05 | Pegasor Oy | Apparatus for monitoring particles in an aerosol |
WO2012098290A1 (en) * | 2011-01-18 | 2012-07-26 | Pegasor Oy | Apparatus and method for monitoring particles |
JP2016048215A (en) * | 2014-08-28 | 2016-04-07 | 株式会社島津製作所 | Electron capture detector and gas chromatograph including the same |
JP2016048214A (en) * | 2014-08-28 | 2016-04-07 | 株式会社島津製作所 | Electron capture detector and gas chromatograph including the same |
-
1984
- 1984-03-31 JP JP6470384A patent/JPS60209167A/en active Granted
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62115657U (en) * | 1986-01-16 | 1987-07-23 | ||
JPH0522860Y2 (en) * | 1986-01-16 | 1993-06-11 | ||
EA018507B1 (en) * | 2008-03-04 | 2013-08-30 | Пегасор Ой | Particle measurement process and apparatus |
WO2009109688A1 (en) * | 2008-03-04 | 2009-09-11 | Pegasor Oy | Particle measurement process and apparatus |
JP2011513742A (en) * | 2008-03-04 | 2011-04-28 | ぺガソー オーワイ | Particle measuring method and apparatus |
EP2247939A4 (en) * | 2008-03-04 | 2012-05-02 | Pegasor Oy | Particle measurement process and apparatus |
US8710849B2 (en) | 2008-03-04 | 2014-04-29 | Pegasor Oy | Particle measurement process and apparatus |
EP2247939A1 (en) * | 2008-03-04 | 2010-11-10 | Pegasor OY | Particle measurement process and apparatus |
CN103354898A (en) * | 2010-12-31 | 2013-10-16 | 皮卡索尔公司 | Apparatus for monitoring particles in an aerosol |
JP2014501391A (en) * | 2010-12-31 | 2014-01-20 | ペガソー オーワイ | A device for monitoring particles in aerosols |
WO2012089924A1 (en) * | 2010-12-31 | 2012-07-05 | Pegasor Oy | Apparatus for monitoring particles in an aerosol |
EA025811B1 (en) * | 2010-12-31 | 2017-01-30 | Пегасор Ой | Apparatus for monitoring particles in an aerosol |
US9683962B2 (en) | 2010-12-31 | 2017-06-20 | Pegasor Oy | Apparatus for monitoring particles in an aerosol |
WO2012098290A1 (en) * | 2011-01-18 | 2012-07-26 | Pegasor Oy | Apparatus and method for monitoring particles |
JP2016048215A (en) * | 2014-08-28 | 2016-04-07 | 株式会社島津製作所 | Electron capture detector and gas chromatograph including the same |
JP2016048214A (en) * | 2014-08-28 | 2016-04-07 | 株式会社島津製作所 | Electron capture detector and gas chromatograph including the same |
Also Published As
Publication number | Publication date |
---|---|
JPH0572540B2 (en) | 1993-10-12 |
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