JPS6223817B2 - - Google Patents

Info

Publication number
JPS6223817B2
JPS6223817B2 JP7290680A JP7290680A JPS6223817B2 JP S6223817 B2 JPS6223817 B2 JP S6223817B2 JP 7290680 A JP7290680 A JP 7290680A JP 7290680 A JP7290680 A JP 7290680A JP S6223817 B2 JPS6223817 B2 JP S6223817B2
Authority
JP
Japan
Prior art keywords
discharge
sample
electrode
graphite
capacitor
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
Application number
JP7290680A
Other languages
Japanese (ja)
Other versions
JPS56168534A (en
Inventor
Isao Fukui
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 JP7290680A priority Critical patent/JPS56168534A/en
Publication of JPS56168534A publication Critical patent/JPS56168534A/en
Publication of JPS6223817B2 publication Critical patent/JPS6223817B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
    • G01N21/67Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges

Landscapes

  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (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, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Description

【発明の詳細な説明】 この発明は鉄鋼などの発光分光分析に多く用い
られるコンデンサスパーク放電形の発光装置に関
するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a capacitor spark discharge type light emitting device that is often used for emission spectroscopic analysis of steel and the like.

従来アルゴンふんいき中での鉄鋼中のC、P、
Sなどを含む多数の元素を同時に定量分析する発
光分光分析装置においては一般に低圧スパーク装
置と称される固定制御ギヤツプ式低圧コンデンサ
放電発光装置がもつとも多く用いられている。こ
の装置は第1図、第2図にその構成の概要を示す
ように主放電コンデンサ1、抵抗器2、インダク
タンス3の選択設定によつて分析に必要な発光条
件を自由に選ぶことができるものである。図中4
は交流電源で通常1000V位の比較的低圧のもの、
5,6はダイオード、7はイグナイタもどり止め
コンデンサ、8は分析ギヤツプで8Pが放電電極
で陽極、8Sが陰極の試料である。9は発光スタ
ンドでアルゴンArを封入している。10はたと
えばシリコンダイオードなどで構成され図示しな
い電源にて作動するイグナイタ回路で11の固定
制御ギヤツプを介して分析ギヤツプ8にトリガス
パークを加え、コンデンサ1の充電電荷Qが放電
電流+iとなつて試料を発光させる。第1図の2
の抵抗器および第2図の6のダイオードが、この
発光装置における放電回路を単一方向性の放電条
件に保持拘束する回路素子であり、その抵抗器2
またはダイオード6に、インダクタンス3に放電
電流+iが流れた直後に発生する逆方向振動電流
を阻止する機能を持たせてある。このため第3図
(横軸tは時間、タテ軸iはスパーク放電々流)
に示すような分析ギヤツプにおけるスパーク放電
が(+)方向だけの波形を形成するものとなり電
極の消耗がなく安定に発光させるものとなつてい
る。しかしながら鉄鋼のうち銑鉄とねずみ鋳鉄
(Si%の多い鋳鉄)は成分中の(C)が黒鉛の形で分
離析出しており、かつガス(主としてO2・空
気)を含んだピンホールが多いため、それらの影
響によつて上記の低圧スパーク装置では正確な分
析ができずやむなく高圧スパーク装置と称するた
とえば18KV位の電圧の放電発光装置に切換えて
分析せねばならる、鉄鋼専門の分析装置において
も、低圧と高圧の2種の発光装置を設けているの
が現状である。
C, P, in steel in conventional argon atmosphere
A fixed control gap type low pressure capacitor discharge light emitting device, generally referred to as a low pressure spark device, is often used in an optical emission spectrometer for simultaneously quantitatively analyzing a large number of elements including S and the like. As shown in Figures 1 and 2, this device allows you to freely select the light emission conditions necessary for analysis by selecting and setting the main discharge capacitor 1, resistor 2, and inductance 3. It is. 4 in the diagram
is an AC power supply with relatively low voltage, usually around 1000V,
5 and 6 are diodes, 7 is an igniter detent capacitor, 8 is an analysis gap, 8P is a discharge electrode and an anode, and 8S is a cathode sample. 9 is a light emitting stand filled with argon. Reference numeral 10 denotes an igniter circuit which is made up of, for example, a silicon diode and is operated by a power supply (not shown). A trigger spark is applied to the analysis gap 8 through the fixed control gap 11, and the charge Q of the capacitor 1 becomes the discharge current +i, and the sample is discharged. to emit light. 2 in Figure 1
The resistor 2 and the diode 6 in FIG.
Alternatively, the diode 6 is provided with a function of blocking a reverse oscillating current that occurs immediately after the discharge current +i flows through the inductance 3. Therefore, Fig. 3 (horizontal axis t is time, vertical axis i is spark discharge current)
The spark discharge in the analytical gap shown in Fig. 1 forms a waveform only in the (+) direction, and the electrodes do not wear out and light is stably emitted. However, among steels, pig iron and gray cast iron (cast iron with high Si%) have (C) in their composition separated and precipitated in the form of graphite, and there are many pinholes containing gas (mainly O 2 / air). Due to these effects, accurate analysis cannot be performed with the low-pressure spark device described above, and analysis must be performed by switching to a high-pressure spark device, for example, a discharge light emitting device with a voltage of about 18 KV. Currently, two types of light emitting devices are provided: low voltage and high voltage.

この発明は以上の現況に鑑みてなされたもので
あり、発光分光分析に従来もつとも汎用されてい
る低圧コンデンサのスパーク放電発光装置が鉄鋼
試料のうちねずみ鋳鉄と鉄鋼材の原料としての銑
鉄の2種だけの分析ができない欠点を解消するに
ついて、放電々極を黒鉛で作り、かつ分析ギヤツ
プの放電極性を反転させ、これと同時に放電方向
を電極から試料への単一方向に拘束している抵抗
またはダイオードを短絡または回路から外す切換
手段を設けることによつて試料分析の直前に黒鉛
を気化し、これによつて試料中またはアルゴン中
の(O2)を(CO)または(CO2)に変換したのち
放電極性が振動現象で電極から試料方向に復帰し
て試料を気化することで含有元素を正確に発光す
るように構成し、すべての鉄鋼試料を低圧スパー
ク装置だけを発光装置として分析しうるものとな
り、分析装置として大巾に簡素化し、低廉化しう
る有効なものの提供を図るものである。
This invention was made in view of the above-mentioned current situation, and the spark discharge light emitting device of a low-voltage capacitor, which has conventionally been widely used for emission spectroscopic analysis, is applicable to two types of steel samples: gray cast iron and pig iron as a raw material for steel materials. To solve the problem of not being able to conduct a single analysis, the discharge electrode is made of graphite, the discharge polarity of the analytical gap is reversed, and at the same time, a resistor or a Vaporize the graphite just before sample analysis by providing switching means to short or remove the diode from the circuit, thereby converting (O 2 ) in the sample or in argon to (CO) or (CO 2 ). After that, the discharge polarity returns from the electrode toward the sample due to a vibration phenomenon, vaporizing the sample, and making it possible to accurately emit light from the contained elements, making it possible to analyze all steel samples using only the low-pressure spark device as a light-emitting device. The aim is to provide an effective analytical device that can be greatly simplified and inexpensive.

以下図面によつてこの発明の実施例を説明す
る。第4図はこの発明の第一の実施例装置の構成
ブロツク図で第1図と同記号のものは説明を省略
する。15,16,17,18の切換開閉器はす
べて連動操作のもので切換制御装置19の作動時
ONする接点が15a,16a,17a,18a
であり、常時(切換制御装置19の非作動時)
ONしている接点が15b,16b,17b,1
8bである。20は放電電極で黒鉛で作られ第1
図の8Pに相当するものである。この構成によつ
て今たとえばねずみ鋳鉄を試料8Sとして発光分
析するばあい19の切換制御装置を作動させる
と、各開閉器の可動接点は図のようにすべてa接
点をONにする。ここで従来装置と同様9のイグ
ナイタ回路10が分析ギヤツプ8にトリガスパー
クを加えると、主放電コンデンサ1の充電電荷Q
は矢印a方向にスパーク放電し、黒鉛電極20を
蒸発気化する。この気化したCが試料8Sないし
は発光スタンド9内の(Ar)中に拡散している
(O2)に結合し(CO)または(CO2)に変換したの
ち、インダクタンス3により発生する逆方向電流
+i′が分析ギヤツプ8を矢印b方向に放電する。
第5図はこの放電電流の波形を示す図で第3図と
同じく横軸tは時間(sec)、タテ軸±iは上記放
電々流−i,+i′を示す。第4図にもどつて上記
a方向の−iが黒鉛電極を気化したのち、インダ
クタンス3が誘起した+i′は第4図では単方向放
電拘束素子である抵抗2が短絡されているので、
第5図のように+i′が振動的に放電するのであ
る。この+i′の正規極性の放電電流によつて試料
8Sすなわちねずみ鋳鉄の蒸発・気化は活発に行
われ、含有元素の発光が正確に測光されるのであ
る。第5図の−i′の半波は主放電コンデンサ1の
放電電流の減衰波であり、再び放電極性が反転し
たもので、僅かに電極を気化するが、問題ではな
い。この約1サイクルの振動する放電々流波形−
i,+i′,−i′は電源4の商用周波数たとえば60Hz
における半サイクルすなわち8.3msecの時間Tの
うち発生するものであり、つぎの半サイクルで1
への充電が行われるので放電は1サイクルごとに
くり返し同一波形で放電され発光されるものとな
る。つぎに第6図によつてこの発明の第二の実施
例装置を説明する。第2図第4図と同記号のもの
は説明を省く。この装置は第2図で示したダイオ
ード6を単方向放電性拘束素子とする放電回路の
もので、切換開閉器18は上記ダイオード6を回
路から切離しと接続を行うもので18aが制御装
置19の作動時ONする。この構成によつてねず
み鋳鉄または銑鉄分析の際、前述の第4図と同様
の作用をし、放電も第5図と全く同じ波形で振動
するものとなる。この第4、第6図の実施例装置
で上記ねずみ鋳鉄が銑鉄以外の鉄鋼の分析の際は
いうまでもないが15,16,17,18の各切
換器の制御装置19をOFFすれば放電回路はす
べて第1、第2図の従来回路構成となり、第3図
に示す単方向性放電が行われるのである。また制
御装置19がなくて各切換器を手動操作してもよ
い。
Embodiments of the present invention will be described below with reference to the drawings. FIG. 4 is a block diagram of the configuration of a first embodiment of the apparatus of the present invention, and the description of the same symbols as in FIG. 1 will be omitted. The switching switches 15, 16, 17, and 18 are all operated in conjunction with each other, and when the switching control device 19 is activated.
The ON contacts are 15a, 16a, 17a, 18a
and always (when the switching control device 19 is not activated)
The ON contacts are 15b, 16b, 17b, 1
It is 8b. 20 is a discharge electrode made of graphite and the first
This corresponds to 8P in the figure. With this configuration, when, for example, gray cast iron is to be subjected to emission analysis as sample 8S, when the switching control device 19 is activated, all the movable contacts of each switch turn on the a contacts as shown in the figure. Here, as in the conventional device, when the igniter circuit 10 of 9 applies a trigger spark to the analysis gap 8, the charge Q of the main discharge capacitor 1
Spark discharge occurs in the direction of arrow a, and the graphite electrode 20 is vaporized. After this vaporized C combines with (O 2 ) diffused in (Ar) in the sample 8S or light emitting stand 9 and is converted into (CO) or (CO 2 ), a reverse current is generated by the inductance 3. +i' discharges the analysis gap 8 in the direction of arrow b.
FIG. 5 is a diagram showing the waveform of this discharge current, and as in FIG. 3, the horizontal axis t represents time (sec), and the vertical axis ±i represents the discharge currents -i, +i'. Returning to FIG. 4, after the -i in the a direction vaporizes the graphite electrode, +i' induced by the inductance 3 is caused by the resistor 2, which is a unidirectional discharge restraining element, being short-circuited in FIG.
As shown in FIG. 5, +i' is oscillatedly discharged. The sample 8S, that is, the gray cast iron, is actively evaporated and vaporized by this +i' normal polarity discharge current, and the luminescence of the contained elements can be accurately measured. The half wave of -i' in FIG. 5 is an attenuated wave of the discharge current of the main discharge capacitor 1, and the discharge polarity is reversed again, and the electrode is slightly vaporized, but this is not a problem. This oscillating discharge current waveform of about one cycle -
i, +i', -i' are the commercial frequency of power supply 4, for example 60Hz
This occurs during a half cycle, that is, a time T of 8.3 msec, and 1 in the next half cycle.
Since charging is performed, the discharge is repeated with the same waveform every cycle, and light is emitted. Next, a second embodiment of the present invention will be explained with reference to FIG. Components with the same symbols as those in FIG. 2 and FIG. 4 will not be explained. This device is a discharge circuit in which the diode 6 shown in FIG. 2 is used as a unidirectional discharge restraint element. Turns ON when activated. With this configuration, when analyzing gray cast iron or pig iron, the same effect as shown in FIG. 4 described above is achieved, and the discharge also oscillates in exactly the same waveform as shown in FIG. 5. When the above-mentioned gray cast iron is analyzed for steel other than pig iron using the apparatus of the embodiment shown in FIGS. All the circuits have the conventional circuit configurations shown in FIGS. 1 and 2, and the unidirectional discharge shown in FIG. 3 is performed. Alternatively, each switch may be manually operated without the control device 19.

以上がこの発明の第一、第二の実施例装置の説
明であるがこの発明は図示や説明に限定されるも
のではなく、たとえば交流電源を簡単のため商用
周波数のもので説明したが、この装置のパワー回
路が低圧であるのでくり返し周波数の高いパルス
波電源としたばあいもこの発明の適用は可能であ
る。またスパーク放電とアーク放電の中間的な特
性をもつ発光装置においても振動条件が満足され
るばあいこの発明は適用できる。また放電方向拘
束手段は低抗・ダイオードに限らずどのような方
法による装置においても適用できることはいうま
でもない。
The above is an explanation of the first and second embodiments of the present invention, but the present invention is not limited to the illustrations and explanations. Since the power circuit of the device is low voltage, the present invention can also be applied when a pulse wave power source with a high repetition frequency is used. The present invention can also be applied to a light emitting device having characteristics intermediate between spark discharge and arc discharge, as long as the vibration conditions are satisfied. It goes without saying that the discharge direction restraining means is not limited to low resistance diodes, but can be applied to devices using any method.

この発明は以上のように構成されているので、
鉄鋼その他の物質の発光分光分析にもつとも広く
用いられている従来の低圧コンデンサ放電発光装
置が鉄鋼のうち銑鉄とねずみ鋳鉄の発光ができな
かつた欠点を解消し、その単方向放電特性を随時
二方向性すなわち放電電流を振動させる新しい着
想によつて試料分析の直前に黒鉛電極を気化させ
上記試料中の(O2)を(CO)または(CO2)にし
て脱酸したのち試料の気化を活溌化して発光さ
せ、従来の高圧スパーク装置と同等の高精度分析
ができることで、鉄鋼専門の分析装置ならば低圧
スパークのこの発明の発光装置だけですべての試
料が分析でき、装置が大巾に簡単化し、かつ操作
容易で低廉になるという大きい効果を奏するもの
となる。
Since this invention is configured as described above,
Conventional low-pressure capacitor discharge light-emitting devices, which are widely used for emission spectroscopic analysis of steel and other materials, have overcome the drawback of not being able to emit light from pig iron and gray cast iron, and can change their unidirectional discharge characteristics to two directions at any time. Based on a new idea of oscillating the discharge current, the graphite electrode is vaporized immediately before sample analysis to deoxidize the (O 2 ) in the sample to (CO) or (CO 2 ), and then the vaporization of the sample is activated. This makes it possible to perform high-precision analysis equivalent to that of conventional high-pressure spark devices, making it possible to analyze all samples using only the low-pressure spark light-emitting device of this invention, making the device much simpler. It has the great effect of being easy to operate and inexpensive.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は従来のイグナイタ付き低圧コンデンサ
放電発光装置のうち単方向放電拘束素子を抵抗器
にしているものの構成ブロツク図、第2図は同じ
く従来装置の単方向放電拘束素子をダイオードに
しているものの構成ブロツク図、第3図は上記従
来装置の放電波形図(単方向性のもの)、第4図
はこの発明の第一の実施例に係る発光分光分析用
発光装置の構成ブロツク図、第5図はこの発明の
実施例装置の選択切換操作時の放電特性の振動波
形図、第6図はこの発明の第二の実施例装置の構
成ブロツク図である。 1……主放電コンデンサ、Q……コンデンサに
蓄積された放電エネルギー(電荷)、2……放電
方向拘束手段の一例としての抵抗器、3……イン
ダクタンス、5……半波整流器(ダイオード)、
6……放電方向拘束手段の一例としてのダイオー
ド、8……分析ギヤツプ、8P,20……放電電
極(20は黒鉛に限定)、8S……分析試料、9
……発光スタンド(アルゴン(Ar)封入)、+i
……単方向性放電電流、−i,−i′……反極性放電
電流、+i′……振動による正方向放電電流、15
……上記2の抵抗を短絡する切換器、16,17
……分析ギヤツプ8における放電極性を反転させ
る切換器、18……上記6のダイオードを回路か
ら切はなす切換器、19……上記各切換器制御装
置、a……電極を気化させる放電方向、b……試
料を発光させる放電方向。
Figure 1 is a block diagram of a conventional low-voltage capacitor discharge light emitting device with an igniter in which a resistor is used as the unidirectional discharge restraint element, and Figure 2 is a block diagram of a conventional device in which the unidirectional discharge restraint element is a diode. 3 is a configuration block diagram of the conventional device described above (unidirectional); FIG. 4 is a configuration block diagram of the light emitting device for emission spectrometry according to the first embodiment of the present invention; FIG. The figure is an oscillation waveform diagram of the discharge characteristic during the selection switching operation of the apparatus according to the embodiment of the present invention, and FIG. 6 is a block diagram of the configuration of the apparatus according to the second embodiment of the invention. 1... Main discharge capacitor, Q... Discharge energy (charge) stored in the capacitor, 2... Resistor as an example of discharge direction restraint means, 3... Inductance, 5... Half-wave rectifier (diode),
6... Diode as an example of discharge direction restraining means, 8... Analysis gap, 8P, 20... Discharge electrode (20 is limited to graphite), 8S... Analysis sample, 9
...Light-emitting stand (argon (Ar) filled), +i
... Unidirectional discharge current, -i, -i'... Opposite polarity discharge current, +i'... Positive direction discharge current due to vibration, 15
...Switcher that short-circuits the above-mentioned 2 resistors, 16, 17
...Switcher that reverses the discharge polarity in analysis gap 8, 18...Switcher that disconnects the diode 6 from the circuit, 19... Control device for each of the above switches, a... Discharge direction that vaporizes the electrode, b ...The direction of the discharge that causes the sample to emit light.

Claims (1)

【特許請求の範囲】[Claims] 1 放電エネルギーをコンデンサに蓄積し、その
蓄積された放電エネルギーによる放電の方向を電
極から試料への単一方向に拘束する放電方向拘束
手段を備えて電極、試料間で放電させ試料を気
化・発光させる装置において、前記電極を黒鉛に
て形成し、かつ、放電エネルギーによる最初の放
電を試料から黒鉛電極への方向に行わせて黒鉛を
気化させるよう前記電極、試料間での放電の極性
を切り換える切換器、および前記放電方向拘束手
段を解除させて試料から黒鉛電極への前記放電に
続いて振動的に黒鉛電極から試料への方向の放電
を行わせ黒鉛の気化ふんい気内において試料を気
化・発光させるよう前記切換器の切換えと同時に
切り換えられる切換器を設けてなり、それら切換
器により単一方向放電と振動放電とを切換え的に
行うようにしたことを特徴とする発光分光分析用
発光装置。
1. A capacitor is equipped with a discharge direction restraining means that stores discharge energy in a capacitor and restricts the discharge direction of the stored discharge energy to a single direction from the electrode to the sample, causing the discharge between the electrode and the sample to vaporize and emit light from the sample. In the apparatus, the electrode is formed of graphite, and the polarity of the discharge between the electrode and the sample is switched so that the first discharge by discharge energy is performed in the direction from the sample to the graphite electrode, and the graphite is vaporized. The switching device and the discharge direction restraining means are released, and following the discharge from the sample to the graphite electrode, the discharge is caused to vibrate from the graphite electrode to the sample, and the sample is vaporized in the graphite vaporization atmosphere. - A light emission for emission spectroscopic analysis characterized in that a switch is provided which can be switched simultaneously with the switching of the switch to emit light, and the switch switches between unidirectional discharge and oscillating discharge. Device.
JP7290680A 1980-05-31 1980-05-31 Discharge type light emitting device Granted JPS56168534A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7290680A JPS56168534A (en) 1980-05-31 1980-05-31 Discharge type light emitting device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7290680A JPS56168534A (en) 1980-05-31 1980-05-31 Discharge type light emitting device

Publications (2)

Publication Number Publication Date
JPS56168534A JPS56168534A (en) 1981-12-24
JPS6223817B2 true JPS6223817B2 (en) 1987-05-25

Family

ID=13502855

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7290680A Granted JPS56168534A (en) 1980-05-31 1980-05-31 Discharge type light emitting device

Country Status (1)

Country Link
JP (1) JPS56168534A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0375782U (en) * 1989-11-24 1991-07-30
JPH0527010U (en) * 1991-03-15 1993-04-06 株式会社オーケーエンジニアリング Ski gloves
JPH06134074A (en) * 1992-10-23 1994-05-17 Kinichiro Yamanaka Ski glove

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0375782U (en) * 1989-11-24 1991-07-30
JPH0527010U (en) * 1991-03-15 1993-04-06 株式会社オーケーエンジニアリング Ski gloves
JPH06134074A (en) * 1992-10-23 1994-05-17 Kinichiro Yamanaka Ski glove

Also Published As

Publication number Publication date
JPS56168534A (en) 1981-12-24

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