EP0377720A1 - Lampe a decharge lumineuse modulee pour spectrometrie par absorption atomique - Google Patents

Lampe a decharge lumineuse modulee pour spectrometrie par absorption atomique

Info

Publication number
EP0377720A1
EP0377720A1 EP19890907695 EP89907695A EP0377720A1 EP 0377720 A1 EP0377720 A1 EP 0377720A1 EP 19890907695 EP19890907695 EP 19890907695 EP 89907695 A EP89907695 A EP 89907695A EP 0377720 A1 EP0377720 A1 EP 0377720A1
Authority
EP
European Patent Office
Prior art keywords
discharge lamp
glow discharge
voltage
volts
emission radiation
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.)
Withdrawn
Application number
EP19890907695
Other languages
German (de)
English (en)
Inventor
Bernhard Bogadin
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.)
Spectruma GmbH
Original Assignee
Spectruma GmbH
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 Spectruma GmbH filed Critical Spectruma GmbH
Publication of EP0377720A1 publication Critical patent/EP0377720A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/10—Arrangements of light sources specially adapted for spectrometry or colorimetry
    • 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
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis
    • 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
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis
    • G01N2021/3114—Multi-element AAS arrangements
    • 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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/069—Supply of sources
    • G01N2201/0696—Pulsed

Definitions

  • the invention relates to a device according to the preamble of claim 1.
  • So-called atomic absorption spectrometry is used for the precise determination of chemical elements, particularly in metal compounds, such as alloys and the like.
  • This takes advantage of the fact that, with a corresponding supply of energy from the outside, electrons of an atom can be raised to an energy-rich orbit and the energy difference which is released when the electron falls back on the original orbit and is emitted to the outside in the form of a light quantum so that the wavelength of the emitted light is specific for each atom.
  • This process takes place in hollow cathode lamps, whereby one-element lamps are generally used to generate an element-specific, monochromatic primary radiation.
  • excitation energy For analysis, it is necessary to add excitation energy to the sample in a suitable form for atomization. This can be done in different ways, for example with the help of flames, thermal plasmas or electrical sputtering processes.
  • Known devices for carrying out atomic absorption spectrometry thus use a hollow cathode lamp for generating an element-specific emission radiation, a burner connected downstream of the hollow cathode lamp for generating a flame which serves as an atom reservoir, an atomizer system for producing aerosols which are fed to the burner and a spectral apparatus as a receiver, which is combined with a suitable data processing system for control and data evaluation.
  • a burner instead of a burner, a graphite furnace for dissolved and solid samples and an atomic source for atomization can also be used to generate the atomic reservoir
  • the object of the invention is to be able to carry out an accurate multi-element analysis in a short time.
  • This object is achieved according to the invention by the features contained in the characterizing part of patent claim 1, expedient developments of the invention being characterized by the features contained in the subclaims.
  • a Grimm glow discharge lamp is used as the device for generating an element-specific emission radiation, which is used and operated as a hollow cathode lamp.
  • this is a glow discharge lamp filled with argon, the cathode of which is sputtered with argon ions.
  • the glow discharge lamp is operated in a modified modulated manner, that is to say
  • REPLACEMENT LEAF a constant voltage is used, on which a pulsating voltage is superimposed. Appropriately, about 50% of the supply voltage is not modulated. The voltage must not drop to zero, since otherwise the lamp would be switched off. A setting time of at least 10 seconds would then be required again.
  • the glow discharge lamp is equipped with targets, which are each composed of several elements. Alloy steel could also be used here. With the glow discharge lamp as the primary light source, atomic absorption spectral analyzes can be carried out on the basis of targets which have, for example, ten different elements and more.
  • the glow discharge lamp is characterized by excellent stability, so that very reliable measurements are possible.
  • the glow discharge lamp operated with a low output of approximately 30 watts can be used practically without limit, and only the targets have to be replaced, but the samples consume thousands of hours due to the low consumption can be used.
  • the distance from the glow layer is reduced only insignificantly and, for example, there is no change in the constant light over a period of 20 minutes, which is responsible for the excellent stability.
  • the glow discharge lamp can be modulated very well when operating with a relatively low power.
  • a conventional hollow cathode lamp consumes very quickly, so that good stability is not guaranteed, and new lamps are required after a short time.
  • the glow discharge lamp is equipped with special multi-element alloys as a target, so that the glow discharge lamp can be operated as a multi-element line radiator.
  • REPLACEMENT LEAF In the subsequent glow excitation, light of several wavelengths is emitted simultaneously. The number of elements is determined by the composition of the target. By selecting a wide variety of mixing ratios, an additional parameter is created in addition to the parameters customary for the glow discharge lamp, such as power, amperage or pressure, as a result of which spectral sensitivity differences can be better compensated for via the target composition. By selecting the composition of the target, the excited elements in the source or atomic reservoir can be matched in a simple manner to the elements to be determined in the samples. Another advantage is the easy change of the target and the associated change in the emitting light composition.
  • Targets for the glow discharge lamp can be produced from metal powder mixtures by remelting or hot isostatic pressing as well as from oxide / metal powder mixtures after densification, e.g. B. by pressing under high pressure.
  • the glow discharge lamp offers far more lines than the conventional hollow cathode lamp, more lines are available per element. This is particularly true for the ultra violet spectral range, which was previously excluded when using hollow cathode lamps.
  • a glow discharge lamp in a device for atomic absorption spectrometry is particularly advantageous where the analytical tasks require the determination of several elements from a solution or sample.
  • alloys that can be used as a glow discharge device, the multi-element radiation can be adapted to the analytical task.
  • a suitable polychromator as many elements can be determined simultaneously as are contained in the target material and still emit sufficient light during sputtering.
  • Another advantage of the measure according to the invention can be seen in the fact that analytical utilization of lines in the ultraviolet range is also possible. This is achieved by keeping the area between the glow discharge lamp and the polychromator under vacuum or flushing it with inert gas, for which purpose a cylindrical tube is expediently used, which extends between the glow discharge lamp and the polychromator and in which the atomic reservoir is also located in particular a graphite furnace. Such an arrangement is practically not possible when using conventional hollow cathodes because the constant change of the hollow cathode makes vacuum operation extremely difficult. With the measures according to the invention, phosphorus and sulfur lines in particular can thus be used analytically.
  • Figure 1 is a schematic view of a device after the invention.
  • Fig. 2 shows an alternative embodiment of the device shown in Fig.l.
  • Fig. 1 shows a purely schematic representation of an apparatus for atomic absorption spectrometry, which has a Grimm glow discharge lamp (1) which is equipped with a target (2).
  • the emitted light beam passes through an atomic reservoir (3), which in the illustrated embodiment is formed by a flame from a plasma torch.
  • a graphite furnace or an atomic source with which solid samples are atomized can also be used for this.
  • the light passing through the flame reaches a polychromator (4) for measuring the lines of the emitted light.
  • the control and data evaluation of the measurement takes place in a data processing system designated (5).
  • a monochromator instead of a polychromator, a monochromator or another
  • the atomic reservoir in the case of FIG. 2 a graphite furnace, is also located inside the tube. With this embodiment, lines in the ultraviolet range can also be detected analytically.

Landscapes

  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Dans un appareil de spectrométrie par absorption atomique, le dispositif de production de radiation d'émission consiste en une lampe à décharge lumineuse de Grimm modulée, qui fonctionne sous une tension pulsée et sous une tension constante superposée à celle-ci.
EP19890907695 1988-07-05 1989-07-03 Lampe a decharge lumineuse modulee pour spectrometrie par absorption atomique Withdrawn EP0377720A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE3822728 1988-07-05
DE3822728 1988-07-05
DE19883827322 DE3827322A1 (de) 1988-07-05 1988-08-11 Geraet zur simultanen atomabsorptionsspektrometrie
DE3827322 1988-08-11

Publications (1)

Publication Number Publication Date
EP0377720A1 true EP0377720A1 (fr) 1990-07-18

Family

ID=25869766

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19890907695 Withdrawn EP0377720A1 (fr) 1988-07-05 1989-07-03 Lampe a decharge lumineuse modulee pour spectrometrie par absorption atomique

Country Status (3)

Country Link
EP (1) EP0377720A1 (fr)
DE (1) DE3827322A1 (fr)
WO (1) WO1990000731A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5125916A (en) * 1991-04-04 1992-06-30 Ras Partnership Stoma cap
DE4401745C2 (de) * 1994-01-21 2003-02-06 Perkin Elmer Bodenseewerk Zwei Verfahren zur Lichterzeugung für die Atomabsorptionsspektroskopie und Atomabsorptionsspektroskopiesystem zur Durchführung des Verfahrens
CN103913225B (zh) * 2013-01-08 2016-04-13 北京瑞利分析仪器有限公司 便携式原子吸收光谱仪的消色差手动调节机构

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB977545A (en) * 1961-12-09 1964-12-09 Hitachi Ltd Improvements relating to the production of hollow cathodes
US3183393A (en) * 1962-04-20 1965-05-11 Westinghouse Electric Corp Discharge device
US3472594A (en) * 1966-06-06 1969-10-14 Philips Corp Multi-channel atomic absorption spectrometer
DE1589389B2 (de) * 1967-06-10 1971-03-18 Grimm. Werner, Dr.rer.nat, 6454 Großauheim Glimmentladungsroehre
AU407994B2 (en) * 1968-05-01 1970-11-06 Commonwealth Scientific And Industrial Research Organisation Improvements in or relating to spectroscopy and colorimetry
US3624447A (en) * 1969-06-25 1971-11-30 Westinghouse Electric Corp Method of operating a high-pressure gaseous discharge lamp with improved efficiency
US3645629A (en) * 1969-07-03 1972-02-29 Technicon Corp Apparatus for spectroscopic analysis with modulated electrodeless discharge tube
JPS503390A (fr) * 1973-05-11 1975-01-14
DE2437704A1 (de) * 1974-08-05 1976-02-19 Beckman Instruments Gmbh Spektrochemischer analysator
JPS5724858B2 (fr) * 1974-11-27 1982-05-26
JPS51111373A (en) * 1975-03-26 1976-10-01 Hitachi Ltd Method and the apparatus to light a lamp for a spectral analyzer
GB2109922B (en) * 1981-11-11 1985-03-20 Philips Electronic Associated Atomic resonance line source lamps and spectrophotometers for use with such lamps
JPS60252242A (ja) * 1984-05-30 1985-12-12 Hitachi Ltd 原子吸光分光光度計
DE3511255A1 (de) * 1985-03-28 1986-10-02 Grün Optik Wetzlar GmbH, 6330 Wetzlar Anordnung zur individuellen regelung der intensitaet mehrer spektrallampen
DE3605911A1 (de) * 1986-02-24 1987-08-27 Ges Foerderung Spektrochemie Glimmentladungslampe sowie ihre verwendung

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9000731A1 *

Also Published As

Publication number Publication date
WO1990000731A1 (fr) 1990-01-25
DE3827322A1 (de) 1990-01-11

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